Geoarchaeology and Archaeological Mineralogy―2021: Proceedings of 8th Geoarchaeological Conference, Miass, Russia, 20–23 September 2021 (Springer Proceedings in Earth and Environmental Sciences) 3031165438, 9783031165436

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Springer Proceedings in Earth and Environmental Sciences

Natalia N. Ankusheva Igor V. Chechushkov  Andrey V. Epimakhov Maksim N. Ankushev Polina S. Ankusheva   Editors

Geoarchaeology and Archaeological Mineralogy—2021 Proceedings of 8th Geoarchaeological Conference, Miass, Russia, 20–23 September 2021

Springer Proceedings in Earth and Environmental Sciences Series Editors Natalia S. Bezaeva, The Moscow Area, Russia Heloisa Helena Gomes Coe, Niterói RJ Brazil, Brazil Muhammad Farrakh Nawaz, Department of Forestry and Range Management, University of Agriculture, Faisalabad, Pakistan

The series Springer Proceedings in Earth and Environmental Sciences publishes proceedings from scholarly meetings and workshops on all topics related to Environmental and Earth Sciences and related sciences. This series constitutes a comprehensive up-to-date source of reference on a field or subfield of relevance in Earth and Environmental Sciences. In addition to an overall evaluation of the interest, scientific quality, and timeliness of each proposal at the hands of the publisher, individual contributions are all refereed to the high quality standards of leading journals in the field. Thus, this series provides the research community with well-edited, authoritative reports on developments in the most exciting areas of environmental sciences, earth sciences and related fields.

Natalia N. Ankusheva · Igor V. Chechushkov · Andrey V. Epimakhov · Maksim N. Ankushev · Polina S. Ankusheva Editors

Geoarchaeology and Archaeological Mineralogy—2021 Proceedings of 8th Geoarchaeological Conference, Miass, Russia, 20–23 September 2021

Editors Natalia N. Ankusheva South Urals Federal Research Center of Mineralogy and Geoecology Ural Branch of the Russian Academy of Sciences (UB RAS) Miass, Russia Andrey V. Epimakhov South Urals State University Chelyabinsk, Russia Polina S. Ankusheva South Urals Federal Research Center of Mineralogy and Geoecology Ural Branch of the Russian Academy of Sciences (UB RAS) Miass, Russia

Igor V. Chechushkov Institute of History and Archaeology Ural Branch of the Russian Academy of Sciences (UB RAS) Ekaterinburg, Russia Maksim N. Ankushev South Urals Federal Research Center of Mineralogy and Geoecology Ural Branch of the Russian Academy of Sciences (UB RAS) Miass, Russia

ISSN 2524-342X ISSN 2524-3438 (electronic) Springer Proceedings in Earth and Environmental Sciences ISBN 978-3-031-16543-6 ISBN 978-3-031-16544-3 (eBook) https://doi.org/10.1007/978-3-031-16544-3 © The Editor(s) (if applicable) and The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 This work is subject to copyright. All rights are solely and exclusively licensed by the Publisher, whether the whole or part of the material is concerned, specifically the rights of translation, reprinting, reuse of illustrations, recitation, broadcasting, reproduction on microfilms or in any other physical way, and transmission or information storage and retrieval, electronic adaptation, computer software, or by similar or dissimilar methodology now known or hereafter developed. The use of general descriptive names, registered names, trademarks, service marks, etc. in this publication does not imply, even in the absence of a specific statement, that such names are exempt from the relevant protective laws and regulations and therefore free for general use. The publisher, the authors, and the editors are safe to assume that the advice and information in this book are believed to be true and accurate at the date of publication. Neither the publisher nor the authors or the editors give a warranty, expressed or implied, with respect to the material contained herein or for any errors or omissions that may have been made. The publisher remains neutral with regard to jurisdictional claims in published maps and institutional affiliations. This Springer imprint is published by the registered company Springer Nature Switzerland AG The registered company address is: Gewerbestrasse 11, 6330 Cham, Switzerland

Contents

Archaeometry in Studies of Archaeological Objects and Sites The Interdisciplinary Research of the Bulgar-Tatar Town of Juketaw . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Nail G. Nabiullin and Rezida Kh. Khramchenkova

3

Preliminary Results of the Strontium Isotopes Analysis in the Framework of the Study of the Mobility of the Bronze Age Population in the Trans-Urals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Andrey V. Epimakhov, Maksim N. Ankushev, Polina S. Ankusheva, Dariya V. Kiseleva, and Igor V. Chechushkov

11

Features of Paleosol Formation as a Key Indicator of Anthropogenic Impacts on Examples of Bronze Age Cultural Layers of the Krasnosamarskoe Settlement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Liudmila N. Plekhanova The Isotopic Signature of Ancient People from the Eneolithic and Bronze Age Interments in the Mountain-Forest Trans-Urals . . . . . . . Olga N. Korochkova, Daria V. Kiseleva, Ivan A. Spiridonov, and Evgeny S. Shagalov Results of Geochemical Research at the Suursuonmäki Early Iron Age Burial Mound . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Mikhail A. Streltcov, Marianna A. Kulkova, and Maria A. Razzak

19

27

35

The Use of Rocks and Minerals by Ancient Societies Mineral Resources of the Jasper Belt of the Southern Urals and Geoarchaeological Objects . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Peter V. Kazakov

47

v

vi

Contents

Stone Products of Prestigious Technologies on the Sites of the Stone and Bronze Age of the Urals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Yu B. Serikov The Microstructure and Mineral Composition of Flint Artifacts at the Epipaleolithic of the Northern Caucasus: Preliminary ESM Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Vladimir A. Tselmovich and Ekaterina V. Doronicheva Ludogorian Flint as an Indicator of Manufacturing Relations Between the Sites of Kodjadermen-Gumelni¸ta-Karanovo VI (Chalcolithic, Bulgaria) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Natalia N. Skakun, Chavdar Nachev, Boryana Mateva, and Vera V. Terekhina Geochemical Data on the North-Western Caucasus Chert Sources and Origin of the Middle Palaeolithic Artifacts . . . . . . . . . . . . . . . . . . . . . . . Ekaterina V. Doronicheva, Marianna A. Kulkova, and Vladimir A. Tselmovitch Geochemical Characterization and Source Identification of Epipaleolithic Chert Artifacts from Psytuaje Rockshelter, North-Central Caucasus: Preliminary Results . . . . . . . . . . . . . . . . . . . . . . . . Vladimir N. Kirillov and Ekaterina V. Doronicheva

55

65

77

87

97

Archaeometric Research of Building Materials of Medieval Stone Structures of the Bolgar Settlement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 111 Rezida Kh. Khramchenkova, Anton N. Kolchugin, Airat G. Sitdikov, and Polina Yu. Kaplan The Mineral Composition of Pigments from the Archaeological Sites of the Early Iron Age Nomads of the Southern Urals . . . . . . . . . . . . . 127 Ksenia G. Margaryan and Anatoly M. Yuminov The Iconographic Canon and Possibilities of the Polovcian Sculptor in Choosing the Stone Type, Style, and Sculpture Processing Technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143 Aleksander V. Yevglevskyy The Construction Material of the Basket from Gonur Depe Administrative and Religious Center (South-Eastern Karakum) . . . . . . . 151 Anatoly M. Yuminov, Larisa Ya. Kabanova, and Natalia N. Ankusheva Scientific Methods in the Study of Ancient Ceramics Formation of Ceramic Traditions of the Late Bronze Age in the Trans-Urals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 163 Stanislav A. Grigoriev and Natalia P. Salugina

Contents

vii

Application of the Method of A. A. Bobrinsky to Study the Brick Paste Composition from Eastern Abkhazian Medieval Temples and Fortresses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 171 Marina E. Klemeshova, Galina V. Trebeleva, Andrey S. Kizilov, Konstantin A. Glazov, Stanislav V. Sokolov, and Gleb Yu. Yurkov SEM Study of Decorative Elements of the Late 3rd Millennium BCE Mosaic from the Royal Tomb No. 3230 of Gonur Depe . . . . . . . . . . . 185 Tatyana V. Yuryeva and Galina E. Veresotskaya Cizhou Ceramics of the Tsarevsky Medieval City in the Collection of the Archaeological Museum of the Kazan University . . . . . . . . . . . . . . . 193 Svetlana I. Valiulina Mining of Ores, Archaeometallurgy and Metalworking Characterization of the Bloomery Iron Slags and Ores from the Zotinsky Ancient Mine, Middle Trans-Urals, Russia . . . . . . . . . . 203 Ivan S. Stepanov, Ivan A. Blinov, and Dmitry A. Artemyev Experience Implementation of Geometric Morphometry in the Study of Volga-Urals Bronze Tools . . . . . . . . . . . . . . . . . . . . . . . . . . . . 219 Egor V. Bersenev and Ilshat I. Bakhshiev Metallurgy and Metalworking in the Late Bronze Age Settlement Near the Gabdrafikovo Village (Orenburg Cis-Urals Territory, Russia) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 227 Ildar A. Faizullin, Vyacheslav V. Trukhanov, Maksim N. Ankushev, and Ivan A. Blinov Iron Metallurgy of Ancient Colchis: The Mineralogical and Geochemical Composition of Slags and Artifacts from the Dzhantukh Site . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 237 Marianna A. Kulkova, Alexander Yu. Skakov, Maya T. Kashuba, Alexander M. Kulkov, and Maryia N. Vetrova The Study of the Early Iron Age Cauldron from the Peschany IV Burial Ground . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 255 A. Yu. Loboda, A. A. Strokov, V. A. Khvostikov, N. V. Leonova, and A. V. Bobylskikh Composition of Non-military Bronze Items from the Kichigino I Burial Ground . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 265 Ivan A. Blinov and Alexander D. Tairov

viii

Contents

Metal Composition of Items of the Early Iron Age from the Collection of the Chesma History and Local History Museum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 275 Irina P. Alaeva, Ivan A. Blinov, Egor O. Vasyuchkov, and Alexander S. Boyarskiy Microstructure and Composition of Obsidian in the Neolithic Collection of the Almalo 1 Locality in Dagestan as an Indication of the Source of Raw Materials and Directions of Cultural Ties . . . . . . . . 283 Vladimir A. Tselmovich Site Analyses and Geographic Information Systems (GIS) in Archaeology The Structure and Layout of the Bronze Age Settlement of Selek (The Southern Urals, Russia) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 295 Ramil R. Nasretdinov, Ilshat I. Bakhshiev, and Roman N. Gabitov Remote Sensing of the Konoplyanka 2 Settlement in the Southern Trans-Urals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 305 Ivan V. Molchanov, Lev A. Muravyev, Denis D. Byzov, and Nikolay V. Soldatkin In Memoriam About the Life and Work of Geophysicist Vladislav V. Noskevich . . . . . . . 315 Natalia V. Fedorova and Lev A. Muravyov

Archaeometry in Studies of Archaeological Objects and Sites

The Interdisciplinary Research of the Bulgar-Tatar Town of Juketaw Nail G. Nabiullin and Rezida Kh. Khramchenkova

Abstract This work features the results of the chemical composition of non-ferrous metal alloys from the archaeological research of the historically famous BulgarTatar city of Juketaw (‘Jukotin’). Archaeological remains of the medieval city (the tenth–fourteenth centuries) are located on the left bank of the Kama River, on the western border of the modern Chistopol city of Tatarstan. The analysis was carried out by the quantitative emission spectral analysis on a diffraction spectrograph DFS458. As a result, four groups of subjects were studied, revealing the features of alloy compositions and raw materials. The first group includes copper items with a maximum content of total impurities of 5% (silver, arsenic, lead, tin). The second group includes items made from a copper alloy with tin and zinc (potin) in the following proportions: Cu 80%: Sn 4–12%: Zn 5–9%. The third group includes items made of tin bronze with the Sn concentration in the alloy of 9–15%. The fourth group includes lead seals; these items are associated with trade. To a certain extent, the alloy composition’s features correlate with the dating of the finds. It is unknown whether the items were made by local artisans or imported. Keywords Bulgar-Tatar Middle Ages · Juketaw · Chemical composition of non-ferrous metal alloys · Quantitative emission spectral analysis

1 Introduction Juketaw is one of the most important and historically famous towns in Volga Bulgaria. Archaeological remains were on the left bank of the Kama River, on the western border of the modern Chistopol city of Tatarstan (Fig. 1). The archaeological complex includes a compactly located group of archaeological sites—the sites of fortified settlements of Juketaw, Donaurovsky I (Krutogorsky), Donaurovsky II settlements, and necropolises. The complex existed for a long time N. G. Nabiullin (B) · R. Kh. Khramchenkova Institute of Archaeology, named after A.Kh. Khalikov, Tatarstan Academy of Sciences, Kazan, Russia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 N. N. Ankusheva et al. (eds.), Geoarchaeology and Archaeological Mineralogy—2021, Springer Proceedings in Earth and Environmental Sciences, https://doi.org/10.1007/978-3-031-16544-3_1

3

4

N. G. Nabiullin and R. Kh. Khramchenkova

Fig. 1 The archaeological complex of Juketaw relatively to Chistopol and Kazan, the Republic of Tatarstan, Russia (1—Juketaw)

(during the tenth-fourteenth centuries), which makes it possible to study materials in dynamics. The Juketaw and Donaurovsky I (Krutogorsky) settlements existed only in pre-Mongol time (layer III); the Donaurovsky settlement had been one of the historical villages in the pre-Mongol time, and it became the main territory of the city of «open type» during the Golden Horde time (layer II). Some research by Juketaw has an adjacent character due to the use of archaeometry techniques (Gazimzyanov and Nabiullin 2011; Petrenko et al. 2012; Asylgarayeva et al. 2014). For example, research materials on the chemical composition of glass products were published by Nabiullin and Khramchenkova (2013). This work has been continued in a series of special studies of pottery production, focusing on sources of clay raw materials (Bakhmatova and Nabiullin 2013; Bakhmatova 2018). Spectral analysis of cast-iron objects has revealed groups with different compositions of micro-admixtures that reflect the characteristics of raw materials (Nabiullin et al. 2017; Shaykhutdinova et al. 2017). Metallographic analyses have been carried out to study the manufacturing technology of forging products using electron microscopy and other studies. Production facilities of ferrous and non-ferrous metallurgy found with bright traces of production (raw materials and blanks, slag and chips, scrap and waste products, etc.) have been identified on the territory of the Golden Horde town of Juketaw. The cultural layer

The Interdisciplinary Research of the Bulgar-Tatar Town …

5

of the settlement is extremely saturated with traces of industrial activity, especially with pieces of slag and small fragments of bricks; in the general complex of cultural remains, tools, and objects of artisans’ labor are significantly presented.

2 Materials and Methods The analysis of the chemical composition of non-ferrous metal alloys was performed by the quantitative emission spectral analysis on a diffraction spectrograph DFS458 in the Restoration and Analytical Department of the Institute of Archaeology named after A. H. Khalikov of the Tatarstan Academy of Sciences (analyst Khramchenkova). This type of analysis allows for determining more than 40 macro-and microelements. The methodology of research of archaeological material by the ESA method is described by Khramchenkova et al. (2016). The chemical composition of 23 finds of non-ferrous metal alloys was investigated. The main part of the items is presumably associated with the Golden Horde time, and it was found on the territory of the Donaurovsky II settlement (Table, No. 12—from the pre-Mongol fortified settlement of Juketaw).

3 Results and Discussion As a result, four groups of subjects were studied, revealing the features of alloy compositions and raw materials. The results of the analyses are shown in Table 1. The first group includes fragments of the dishes, bracelet, hook, Christian body small cross, cooper plates, and rods with a maximum content of total impurities (Ag, As, Pb, Sn) of 5% (Table 1, Nos. 1–13; 13 copies); a separate subgroup includes objects with a higher As the concentration of 0.5–0.9% (Table 1, Nos. 1–4; 4 items). The second group includes trim of belt, bracelet, copper plate, and rod made from an alloy of Cu with Sn and Zn (potin) in the proportions of Cu 80%: Sn 4–12%: Zn 5– 9% (Table 1, Nos. 14–17; 4 items). The third group includes bracelets, belt buckles, and trim of belts made of Sn bronze with an Sn concentration in the alloy of 9–15% (Table 1, Nos. 18–20; 3 items). The fourth group includes lead seals; these items are associated with trade (Table 1, Nos. 21–23; three items, four analyses). The first, second, and third groups include items with different functional purposes; scraps of cooper plates and rods associated with the production and repair of products. The finds of the third group made of tin bronze contain items that allow for dating: a lamellar bracelet (Table 1, No. 18; type A-Ib-1 according to Polyakova) (1997, p. 180, fig. 62, 2). and trim of a belt (Table 1, No. 20; type B-III-1 according to Polyakova) (1997, p. 207, fig. 67, 5) of the Golden Horde time and a lyre-shaped belt buckle (Table 1, No. 19; type IB1 according to Kazakov), widespread in pre-Mongol times from the beginning of the tenth century (Kazakov 1991, p. 129).

Handle of the dishes

Cooper plate

Cooper plate

Cooper plate

Fragments Donaurovsky of the II settlement dishes

Bracelet

Cooper plate

Hook

Cooper plate

Body small cross

2

3

4

5

6

7

8

9

10

11

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Handle of the dishes

1

I

II

II

II

II

II

II

II

II

II

II

0.49

As

0.49

0.53

0.098

0.15

0.0051 0.002

0.0028 0.083

0.024

0.011

0.0066 0.083

0.0009 0.033

0.015

0.012

0.0011 0.89

0.014

Al

0.039 0.0021 0.062

0.24

0.44

0.84

0.36

0.37

0.48

0.51

0.79

0.59

0.53

Archaeological Layer Ag site

Item

№

Cu

Fe

Mn

Ni

0.0003 98.1 0.01 0.01 0.014

0.0002 98.3 0.01 0.01 0.026

0.0003 94.1 0.02 0.01 0.022

0.0003 96.3 0.03 0.01 0.011

0.0004 95.7 0.02 0.01 0.021

0.0001 93.3 0.03 0.01 0.027

Co

0.31

0.18

0.15

3.58

0.58

0.23

3.75

P

0.0002 97.8 0.03 0.01 0.015

0.12

0.029

0.0001 97

0.02 0.01 0.019

0.02

0.0051 0.0002 95.5 0.03 0.01 0.0013 2.93

0.016

0.0095 0.0009 96.4 0.01 0.01 0.0045 0.45

0.0078 0.0005 97.7 0.02 0.01 0.012

0.012

0.022

0.086

0.021

0.038

0.007

Bi

Table 1 Chemical composition of non-ferrous metal alloys from the City of Juketaw Si

Sn

Sb

0.0082

0.0028

0.0074

0.0033

0.0003

Au

0.0063

0

(continued)

0.0043

0.039

0.01 0.0078

0.01 0.0091

0

0.01 0.011

0

0

0

0

0

Zn

0.0018 0 0.47 0.17 1.58 0.22

0.73 0.45 0

0.99 0.16 0.02 0.25

0.87 0.96 0.07 0.17

0.63 0.25 0.11 0.33

0.28 0.49 0.04 0.29

0.42 0.13 0.03 0.35

0.39 0.39 0.02 0.34

0.48 0.87 0.02 0.28

1.84 0.25 0.01 0.32

0.92 0.51 0.01 0.34

Pb

6 N. G. Nabiullin and R. Kh. Khramchenkova

Donaurovsky II settlement

Trim of belt

Bracelet

Rod

Cooper plate

Bracelet

Belt buckle

Trim of belt

Seal

Seal

14

15

16

17

18

19

20

21

22

23a Seal

23b

Donaurovsky II settlement

Rod

13

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Donaurovsky II settlement

Rod fortified (bracelet?) settlement

12

I

I

I

I

III

II

II

III

II

I

I

I

0.097

0.003

0.0007 0.031

0.36

0.19

0.0057 0.039

0.0037 0.13

0.048

0.0002 0.033

0.0007 0.17

Cu

Fe

Mn

0.011

0.012

0.08

0.03

0.93

0.009

0.016

0.0015 0.0024 0.0001 0.01 0.01 0

0.31

0.0002 0

Si

Sb

0.05 0.44

Sn

99.4

99.6

1.2

96.9

0.1

0

0.16 2.77 0.0031 0

0.0014

0

0

0

0.07 0.0038

0.01 0

0.01 0.0044

7.79 0.013

8.65 0.0022

5.11 0.15

0.33 2.28 0.0017 0

0.22 0.2

0.0011

0.0013

Au

9.18 0.0007

0

0

Zn

0.13 0.17 0.0007 0

1.02 10.4 0.092

3.02 0.79 9.31 0.057

1.95 0.16 15.1 0.19

0.56 0.13 11.9 0.023

0.74 0.18 6.14 0.097

0.92 1.02 4.01 0.08

0.74 0.24 6.42 0.5

0.28 0.03 0.12 0.22

0.62 0.2

Pb

0.0002 0.03 97.2

0.0011 0

0.0004 0

0.0016 86.5 0.16 0.02 0.013

0.0005 83.6 0.22 0.01 0.0009 2.46

0.0089 0.0027 81.5 0.03 0.01 0.0063 0.74

0.18 0

0.0002 0.0086 0.0046 0.0003 0.05 0.01 0 0.002

0.06

P

0.0059 0.02

0.0016 82.7 1.01 0.01 0.017

0.0048 84.7 0.14 0

0.0009 82.5 0.04 0

0.0058 0.0044 79

0.032

0.03

0.014

0.078 0.0007 0.0013 0.0032 0.0002 0.02 0.01 0

0.12

0.42

Ni

0.0001 98.2 0.01 0.01 0.023

Co

0.0042 0.0006 98.6 0.01 0.01 0.0168 0.03

0.041

Bi

0.009 0.0056 0.0001 0.0001 0.0001 0.02 0.01 0

0.12

As

0.0004 0.14

Al

0.035 0.038

0.11

0.25

0.24

2.73

0.22

0.22

0.19

Archaeological Layer Ag site

Item

№

Table 1 (continued)

The Interdisciplinary Research of the Bulgar-Tatar Town … 7

8

N. G. Nabiullin and R. Kh. Khramchenkova

The belt buckle stands out among the Golden Horde items of the first group, particularly by the high content of lead. It is possible that, in this case, the features of the alloy composition, to a certain extent, correlate with the dating of the finds. Simultaneously, the chemical analysis of a rod (a bracelet?) from the first group, presumably repositioned from the pre-Mongol layer of the fortified settlement of Juketaw (Table 1, No. 12), did not reveal any features that allow for distinguishing it in this group from the objects of the Golden Horde time. It is unknown whether the items were made by local artisans or imported. A small Christian body cross is a foreign cultural object (the first group; it differs by the increased content of Sn).

4 Conclusions 1. The features of the alloy composition correlate with the dating of the finds to a certain extent. 2. Currently, there is no clear answer to the question: do the items have a local or imported origin? 3. Despite the existence of non-ferrous metallurgy on the territory of the Golden Horde city of Juketaw, little is known about it, including cuprous sandstone, a locally available raw material. 4. There is no data on the pre-Mongol time’s metallurgy and metalworking. It seems that continued studies of the chemical composition of representative samples of reliably stratified archaeological finds from non-ferrous (and precious) metal alloys will make it possible to refine the characteristics of the formulation and raw material regarding the time of production and existence. Based on these and subsequent studies, it is planned to create a database to help identify the features of craft traditions of the different historical periods of the Bulgar-Tatar Middle Ages.

References Asylgarayeva, G.Sh., Bakhmatova, V.N., Gazimzyanov, I.R., Melnikov, L.V., Nabiullin, N.G., Mukhametshin, D.G., Semykin, Y.A., Khramchenkova, R.Kh.: Itogi i perspektivy issledovaniy Dzhuketau (The results and prospects of research of Juketaw). In: Materialy IV (XX) arkheologicheskogo s”yezda (The Materials of the IVth (XXth) archaeological Songress). 20–25 oktyabrya 2014 g. Tom III. Kazan, 444–446 (2014) (in Russian) Bakhmatova, V.N., Nabiullin, N.G.: Istochnikovyye vozmozhnosti nepolivnoy glinyanoy «traditsionnoy» posudy (na primere keramicheskogo kompleksa goroda Dzhuketau X–XIV vv.) (Possible origins of the unglazed «traditional» pottery (exemplified by Juketaw ceramic site of the 10th–14th centuries). Filologiya i kul’tura (Philology and Culture) 3(33), 232–235 (2013) (in Russian) Bakhmatova, V.N., Nabiullin, N.G.: Tekhnologicheskoye izucheniye «prikamsko-priural’skoy» keramiki iz domongol’skikh kompleksov Dzhuketau (Technological study of “Kama-Urals”

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ceramics from pre-mongol complexes of Juketaw). Povolzhskaya arkheologiya (The Volga River Region Archaeology) 1(23), 253–274 (2018) (in Russian) Gazimzyanov, I.R., Nabiullin, N.G.: Antropologiya naseleniya Dzhuketau (po materialam Donaurovskogo nekropolya) (Anthropology of the Population of Juketaw (On the Materials of Donaurovskii Cemetery). In: Uchenye Zapiski Kazanskogo Universiteta. Seriya Gumanitarnye Nauki (Proceedings of Kazan University. Humanities Series), vol. 153, book 3, pp. 21–28 (2011) (in Russian) Kazakov, Ye.P.: Bulgarskoye selo X–XIII vv. nizoviy Kamy (Bulgar village of the 10th–13th centuries in the lower reaches of the Kama), p. 176. Tatknigoizdat Publ, Kazan (1991) (in Russian) Khramchenkova, R., Degryse, P., Sitdikov, A., Kaisin, A.: Analytical studies of post medieval glass bottle marks from excavations at Kazan Kremlin (Russia). J. Archaeol. Sci. Rep. 12, 25–27 (2016) Nabiullin, N.G., Khramchenkova, R.Kh.: Steklyannyye ukrasheniya Dzhuketau: morfologiya i khimicheskiy sostav (Glass jewelry of Juketaw: morphology and chemical composition). Filologiya i kul’tura (Philology and Culture) 3(33), 240–244 (2013) (in Russian) Nabiullin, N.G., Belyayev, A.V., Khramchenkova, R.Kh., Shaykhutdinova, Ye.F., Yanbayev, R.M.: Chugunnaya posuda Dzhuketau: rezul’taty mezhdistsiplinarnykh issledovaniy (Cast iron dishware from Juketaw: preliminary interdisciplinary research results). Povolzhskaya arkheologiya (The Volga River Region Archaeology) 2(20), 42–58 (2017) (in Russian) Petrenko, A.G., Asylgarayeva, G.SH., Nabiullin, N.G.: Khozyaystvennaya deyatel’nost’ naseleniya goroda Dzhuketau po dannym arkheozoologicheskikh materialov (Economic activity of Juketaw population according to archeozoological materials). Filologiya i kul’tura (Philology and Culture) 2(28), 274–281 (2012) (in Russian) Polyakova, G.F.: Izdeliya iz tsvetnykh i dragotsennykh metallov (Wares from non-ferrous and precious metals). In: Gorod Bolgar: Remeslo metallurgov, kuznetsov, liteyshchikov (Bolgar city: craft of metallurgists, blacksmiths, casters), pp. 269–298. The Institute of Language, Literature and History named after G. Ibragimov Publ., Kazan (1996) (in Russian) Acta IMEKO 6(3), 87–93 (2017). https://repository.kpfu.ru/?p_id=167555 Shaykhutdinova, E., Khramchenkova, R., Nabiullin, N., Belyaev, A., Yanbaev, R., Sitdikov A.: Interdisciplinary research of iron casting technologies in the town of Juketaw during the golden horde period. In: Acta IMEKO 6(3), 87–93 (2017)

Preliminary Results of the Strontium Isotopes Analysis in the Framework of the Study of the Mobility of the Bronze Age Population in the Trans-Urals Andrey V. Epimakhov, Maksim N. Ankushev, Polina S. Ankusheva, Dariya V. Kiseleva, and Igor V. Chechushkov Abstract The paper presents preliminary results of studying ancient mobility in the southern Urals by applying the strontium analysis. In total, 70 points were sampled, covering 33.000 km2 . We measured the 87 Sr/86 Sr ratio in 67 samples of water and 57 samples of grass from the same locations. The statistical analysis of the two batches demonstrates their close similarity. The map of values was interpolated with simple kriging based on the 67 samples of water. The map demonstrated the variability in values depending on the geological structure of the region. Keywords Strontium isotope analysis · Migration · Sintashta · Southern Urals

1 Introduction The study of mobility in archeology is stimulated from the outside. There are two factors. The first is traditionally high importance of this topic in other disciplines (geography, economics, urban studies, etc.) that lead to the development of a general mobility theory. Sheller and Urry (2006) have even suggested that there is a development of a new methodological paradigm. The second factor is the development of new methods for studying mobility in the past. At the same time, the topic was in the sphere of interest of many scholars, who relied on typology as the primary tool to study mobility and migration. Currently, the range of methods is significantly expanded by applying paleo-DNA and geochemistry (Vandkilde et al. 2015; A. V. Epimakhov (B) · D. V. Kiseleva South Ural State University, Chelyabinsk, Russia e-mail: [email protected] M. N. Ankushev · P. S. Ankusheva Institute of Mineralogy SU FRC MG UB RAS, Miass, Russia D. V. Kiseleva Institute of Geology and Geochemistry UB RAS, Ekaterinburg, Russia I. V. Chechushkov Institute of History and Archaeology UB RAS, Ekaterinburg, Russia © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 N. N. Ankusheva et al. (eds.), Geoarchaeology and Archaeological Mineralogy—2021, Springer Proceedings in Earth and Environmental Sciences, https://doi.org/10.1007/978-3-031-16544-3_2

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etc.). Some methods are devoted to reconstructing large-scale, long-distance movements. The other methods help to turn to smaller-scale processes, such as individual, seasonal, economic, and other types of mobility. Resolving these issues aims at reconstructing and understanding economic and social phenomena, especially given that most such reconstructions are based on settlement studies, sometimes combined with studies of synchronous funerary sites. All of the above is directly related to the study of the Trans-Ural Bronze Age (3rd– 2nd millennia BCE). This steppe and forest-steppe zones of this area are relatively well studied, and numerous sites (settlements, burial grounds, ancient mines, etc.) have been discovered. Several archaeological cultures have been attributed, and their relative chronologies have been established. The economy based on complex animal herding and other industries, including metal production, is well recognized. The variability of the geological structure is one of the critical factors for applying the 88Sr/86Sr radiogenic isotope method. The Urals fully meet this criterion. The lack of natural values of strontium isotope variations is an obstacle for mobility studies. On the one hand, the method has been successfully applied in the Urals (Kiseleva et al. 2019; Ankusheva et al. 2021; etc.). On the other hand, researchers have focused on specific loci where natural samples were purposefully collected. The same approach is also typical outside the Urals, but it seems insufficient if we attempt to look at a larger historical picture. Our goal at this stage is to interpolate a base map of the strontium isotopes of the southern Trans-Urals, comparing it to the major geological structures of the region. This involves the development of a sampling methodology and analyzing various samples (rocks, water, mollusk shells, soil, and plants of the same species) gathered at the same location.

2 Materials and Methods The sampling area lies north of the Ui River, along the border of the Chelyabinsk region of Russia, with the Republic of Kazakhstan in the east. In the west, it enters the Republic of Bashkortostan of Russia. In the south, it touches the Orenburg region of Russia (Fig. 1). For sampling, 70 points were located in the grid at 25 km one from another. Samples were collected within 5-km-radius buffer zones around these 70 points. The sample points were located at the maximum possible distance from industrially active settlements, cultivated fields, and farmland, where fertilizers can serve as a potential source of strontium with a modified isotopic composition (Thomse and Andreasen 2019; Maurer et al. 2012). The sampling map covers the distribution zone of the Sintashta-Petrovka sites of the southern Trans-Urals. The sampling zones intersect well with the 10-km-radius buffer zones of several Late Bronze Age reference settlements (such as Kamennyi Ambar, Arkaim, Sintashta, Levoberezhnoe, Sarym-Sakly, Stepnoye, Chernorechie). The radius of 10 km was chosen to cover plausible ancient economic activity zones, as the residents of the Sintashta-Petrovka settlements probably needed an area with a radius of at least 4 km for pasturing (Stobbe et al. 2016).

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Fig. 1 Map of the study area and sampling area (UTM zone 41)

To date, samples from two series have been studied: the samples of water (n = 67) and the samples of wild plants (Artemísia absínthium) (n = 57), allowing for preliminary conclusions. The analysis corresponds to the following research stages: (1) determination of strontium isotopic values in samples, (2) statistical analysis, (3) strontium map interpolation, and (4) analysis of the strontium spatial distribution. Measurements of strontium were carried out in a cleanroom unit (classes 6 and 7 of the ISO, the Center for collective use “Geoanalyst,” the Ural Branch of the Russian Academy of Sciences, Ekaterinburg). Plant samples were air-dried, ground in an electric mill, and carbonized for 12 h (Maurer et al. 2012). Water samples were preserved with concentrated nitric acid and, after filtering and determining the strontium content, were sent directly to the chromatographic separation of Sr, which was carried out on SR resin (TrisKem) according to the one-stage scheme (Muynck et al. 2009; Kasyanova et al. 2019). The 88 Sr/86 Sr isotope composition was measured on a Neptune Plus magnetosector multi-collector mass spectrometer with inductively coupled plasma (MCICP-MS). Mass discrimination was corrected using a combination of bracketing and normalization according to the exponential law: 88 Sr/86 Sr = 8.375209 (Nier 1938). The results were further bracketed using the NIST SRM 987 strontium carbonate isotope standard by an average deviation from the reference value of 0.710245 (according to the GeoReM database, http://georem.mpch-mainz.gwdg.de/) for every two samples taken between NIST SRM 987 measurements. To control measurements

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of the strontium isotope composition, the NIST SRM 987 isotope standard was regularly measured over a long time (during 2019–2020): 87 Sr/86 Sr = 0.71025, 2SD = 0.00012 (104 measurements in two parallels). The uncertainty under conditions of intralaboratory reproducibility (2σ) for NIST SRM-987 was ±0.003%.

3 Results and Discussion 3.1 Statistical Analysis of Sample Values from Water and Plant Samples The batch of water samples consists of 67 values. The range of values is 0.008571 at min = 0.707308, max = 0.715879. The stem-and-leaves plot is bell-shaped, singlepeaked, and has a slight upward inclination, close to being normally distributed. Therefore, the numerical series can be statistically examined and characterized in terms of mean values for subsequent comparison with other types of samples. The water sample is characterized by the following statistical values: mean is 0.709525, SD is 0.001018, SE (95%) = 0.000492, i.e., the mean value lies in the range from 0.709279 to 0.709771 (0.709525 ± 0.000492) at the 95% confidence level. The batch of plant samples consists of 57 values. The range of values is 0.00321 at min = 0.707972, max = 0.711182. The stem-and-leaves plot is bell-shaped and single-peaked, close to being normally distributed. The grass sample is characterized by the following statistical values: mean is 0.709602, SD = 0.000532, SE (95%) = 0.709460, i.e., the average value lies in the range from 0.709460 to 0.709743 (0.709602 ± 0.709460) at the 95% confidence level. The two batches have similar characteristics, and a comparison with the t-test shows no statistically significant difference between the means (t = 0.513298, p = 0.608664). This may indicate a slight local variability in the measured values of two different types of samples. To test this hypothesis, we compare the difference between the measured values of pairs of samples obtained within the same buffer zone. Thus, the difference varies from −0.002073 to 0.005164, with an average value of 0.000008 and a standard deviation of 0.000898. This average difference is insignificant because close to the two-sigma deviation of the measured values (0.000007). Visual analysis of the mapped values also confirms the similarities of local measurements of plant and water samples.

3.2 Mapping of Strontium Values The resulting map of the distribution of strontium isotopes in the water samples shows a spatial pattern: values increase from west to east, with the highest values in the

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Trans-Ural0 peneplain zone (Fig. 2). The identified distribution in the 87Sr/86Sr ratios coincides with four large structural-formational zones of the Trans-Urals, which differ from each other in the genesis, age, and composition of the constituent rocks. In the west, the sampling grid covers the Central Ural megazone, composed of metamorphosed deposits of the Upper Precambrian—Lower Paleozoic ages (Fig. 2) (Puchkov 2000). The range of rocks includes catagenetically altered sedimentary sequences and highly metamorphosed crystalline complexes. The megazone was sampled at only two locations on the edge of the sampling area (Fig. 2), so expanding the grid to the west is necessary. The Magnitogorsk megazone is formed by Paleozoic island-arc volcanic-sedimentary formations lying to the east. Low values of 87 Sr/86 Sr characterize the zone. A high 87 Sr/86 Sr value in the NW corner of the grid needs additional study. Further east, the grid overlays the East Ural megazone, a collage of microcontinental blocks dissected by ophiolite and island arc formations. Ultramafic complexes, granite intrusions, volcanic-sedimentary sequences, and metamorphic complexes contribute to the complex geological structure of the zone. The zone is characterized by the highest values of 87 Sr/86 Sr. The eastern boundary of the sampling area lies within the Trans-Ural megazone. This megazone is composed of Carboniferous paleoisland-arc calc-alkaline formations. The megazone has been tested by a few

Fig. 2 Map of 87 Sr/86 Sr isotope distribution based on water samples with geological structuralformational zones of the study area

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points and needs further sample expansion. So far, the Trans-Ural megazone demonstrates average values of 87 Sr/86 Sr. Given the complex geological structure and the broadest range of rocks in the study area, a positive result is the low differentiation of the identified anomalies. Due to this, the described technique demonstrates its suitability for studying sublatitudinal migrations of the ancient population within the Southern Trans-Urals. The map of bioavailable strontium is interpolated with the use of geostatistical methods. Fundamentally, geostatistical methods proceed from the idea of obtaining values of unknown points by interpolating data from known points. Kriging is one of the interpolation methods widely used in topography, cartography, and geology. This method is based on the assumption that at least some spatial variations can be modeled using spatial autocorrelation (the tendency for similar values of spatially close objects, in this case, the measured values of Sr isotopes) (Oliver 1990). During interpolation, the algorithm selects a weighted average of the sample values with minimum variance (Armstrong 1998, p. 88). Kriging techniques can describe and model spatial structural patterns, predict unmeasured point values, and measure the uncertainty associated with a predicted value at unmeasured locations. The method is also suitable for determining unknown values if there is a directional bias in the data. As a result, a surface model can be represented by two-dimensional maps or three-dimensional models. We applied normal kriging (kriging with an unknown mean) with a linear variogram. The choice of interpolation method seems to be justified since we can assume that our data possess two fundamental characteristics: autocorrelation and spatial bias. The cell size of the interpolated map is 5 km by 5 km (Fig. 3).

4 Conclusions As a result, it has been found that the distribution of strontium isotope values from the water and plant samples have similar spatial patterns. The statistical differences between mean values are insignificant. A map of strontium isotope values was interpolated for an area of 33,000 km2 based on 67 water samples (Fig. 3). According to this map, there is a general trend of increasing values from the west to the east. The zone of high values is located submeridionally, apparently confined to the East Ural megazone. The zone of low values inclines towards the Magnitogorsk megazone. A significant expansion of the survey area is necessary to specify isotopic values of other tectonic zones, covered with only a few sampling points (the Central Ural and Transural megazones, the West Siberian Plate). In addition, the map revealed the need to supplement the number of analyzes within the boundaries of the surveyed area in cases where the interpolation is based on single analyzes or near the boundary of geological structures. Despite the intermediate nature of our results, it can be stated that the data meet our expectations and can be used to diagnose the local versus non-local origin of biological organisms. In the next stage of our work, we aim to measure strontium isotope

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Fig. 3 Interpolated map of 87 Sr/86 Sr isotope based on water samples

values of samples originating from the Late Bronze Age sites, thereby determining the degree of mobility of people and animals. Acknowledgements The study was financially supported by the Russian Science Foundation, project No. 20-18-00402 “Migrations of human groups and individual mobility in the framework of a multidisciplinary analysis of archaeological information (the Bronze Age of the Southern Urals).”

References Ankusheva, P.S., Kiseleva, D.V., Bachura, O.P., Alaeva, I.P., Ankushev, M.N., Okuneva, T.G.: Labor and Food of Bronze Age Miners in the Southern Trans-Urals (based on the strontium isotopic composition in the Novotemirsky mine osteological remains). Stratum plus 2, 69–83 (2021). (in Russian) Armstrong, M.: Basic Linear Geostatistics, 154 p. Springer Science & Business Media (1998)

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Kasyanova, A.V., Streletskaya, M.V., Chervyakovskaya, M.V., Kiseleva, D.V.: A method for 87 Sr/86 Sr isotope ratio determination in biogenic apatite by MC-ICP-MS using the SSB technique. AIP Conf. Proc. 2174(1), 020028 (2019) Kiseleva, D.V., Chervyakovskaya, M.V., Shishlina, N.I.: Isotopic analysis of strontium in modern raw materials and fossil textiles. Geoarchaeol. Archaeol. Mineral. 25–28 (2019) (in Russian) Maurer, A.-F., Galer, S.J.G., Knipper, C., Beierlein, L., Nunn, E.V., Peters, D., Tütken, T., Alt, K.W., Schöne, B.R.: Bioavailable 87 Sr/86 Sr in different environmental samples—Effects of anthropogenic contamination and implications for isoscapes in past migration studies. Sci. Total Environ. 433, 216–229 (2012) Muynck, D.D., Huelga-Suarez, G., Heghe, L.V., Degryse, P., Vanhaecke, F.: Systematic evaluation of a strontium-specific extraction chromatographic resin for obtaining a purified Sr fraction with quantitative recovery from complex and Ca-rich matrices. J. Anal. Spectrom. 24, 1498–1510 (2009) Nier, A.O.: The isotopic constitution of strontium, barium, bismuth, thallium and mercury. Phys. Rev. 54, 275–278 (1938) Oliver, M.A.: Kriging: a method of interpolation for geographical information systems. Int. J. Geograph. Inf. Syst. 4, 313–332 (1990) Puchkov, V.N.: Paleogeodinamika Yuzhnogo i Srednego Urala (Paleogeodinamics of the Southern and Middle Urals), 146p. Dauriya, Ufa (2000) (in Russian) Sheller, M., Urry, J.: The new mobilities paradigm. Environ. Planning a: Economy Space 38(2), 207–226 (2006) Stobbe, A., Gumnior, M., Rühl, L., Schneider, H.: Bronze Age human–landscape interactions in the southern Trans-Ural steppe, Russia-Evidence from high-resolution palaeobotanical studies. The Holocene 26(10), 1692–1710 (2016) Thomsen, E., Andreasen, R.: Agricultural lime disturbs natural strontium isotope variations: implications for provenance and migration studies. Science Advances 5(3), eaav8083 (2019) Vandkilde, H., Hansen, S., Kotsakis, K., Kristiansen, K., Müller, J., Sofaer, J., Sørensen, M.L.S.: Cultural mobility in Bronze Age Europe. In: Suchowska-Ducke, P., et al. (eds.) Introduction Mobility of Culture in Bronze Age Europe, pp. 5–37 (British Archaeological Reports, S2771). Oxford, GB. Archaeopress (2015)

Features of Paleosol Formation as a Key Indicator of Anthropogenic Impacts on Examples of Bronze Age Cultural Layers of the Krasnosamarskoe Settlement Liudmila N. Plekhanova Abstract The cultural layers of ancient (3rd–2nd millennia BCE) settlements are unique study objects. Top-down, they consist of modern-day soils overlapping the ancient buried soil, strongly altered by anthropogenic pressure. Cultural layers always contain the remains of artifacts and human life in the settlement, such as bones and ceramics. Settlement sites contain cultural layers that are a promising object for studying the ancient anthropogenic mineral formation. Still, such studies should follow the study of the principal physical and chemical properties of soils. Soils of a Bronze Age settlement were studied along with the natural soils of the floodplain terrace of the Volga river, which form a common area with the terrace of the Samara River. Paleourbanozems (soils formed on cultural layers of ancient settlements) with anthropogenic horizons built into the system of natural soil horizons are formed on the settlement site. The Krasnosamarskoe settlement revealed two generations of solonetzic soils located one above another and differing in the thickness of solonetzic jointing (including thin-columnar solonetzic soils). These solonetzic soils were formed during various stages of the Bronze Age, but subsequently, they morphologically merged into a single horizon. The author investigated the stages of soil cover formation of river valleys in connection with the long-term anthropogenic impact with a specific focus on the Bronze Age societies of the Samara Volga region. Keywords Paleosols · Bronze Age · Climate aridization · Solonetz

1 Introduction Modern soil science considers that the ancient anthropogenic impact, whether it was the soil cultivation, the construction of settlements, or grazing, in most cases leads to the degradation of the surrounding landscapes. The accumulation rate of anthropogenic “sediments” during the formation of the thick cultural layers is akin L. N. Plekhanova (B) Institute of Physicochemical and Biological Problems in Soil Science of the Russian Academy of Sciences, Pushchino, Russia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 N. N. Ankusheva et al. (eds.), Geoarchaeology and Archaeological Mineralogy—2021, Springer Proceedings in Earth and Environmental Sciences, https://doi.org/10.1007/978-3-031-16544-3_3

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to geological processes typical of the alluvial-diluvial sediments. Cattle breeding and the development of ancient mines have an even greater impact. They have been developing in the steppe belt of Eurasia since the Bronze Age (3rd–2nd millennia BCE). The tasks of my soil-archaeological research are: to understand the patterns of soil evolution in various biogeographic regions; to establish the direction and rate of the variability of soil properties and processes relative to the climate dynamics in the Holocene (based on buried paleosols under mounds, settlements, defensive ramparts) within the period from the 3rd millennium BCE until the nineteenth century CE. These aims can be achieved based on assessing the degree of human impact on the soil cover and landscapes during various historical periods. Currently, we have accumulated considerable experience in studying anthropogenically transformed soils with various degrees of transformation, where a new horizon is built into the system of natural soil horizons (Demkin et al. 2012; Golyeva et al. 2018; Sedov et al. 2010; Kashirskaya et al. 2019; Plekhanova and Tupakhina 2021, etc.). Special attention should be paid to recording the accelerated mineral formation under various anthropogenic impacts. The activity of specific soil microorganisms caused by increased humidity and temperature resulted in the increased content of ferromagnetic (magnetite, maghemite) (Plekhanova 2021). As a result, the magnetic susceptibility of soils increases, both in soils of cold soil-climatic facies and in steppe soils. The reference sections from the Voronezh region of Russia containing the Late Pleistocene soils display increased aggregation and accumulation of carbonates, humates, and fulvates of calcium, changing the morphology of secondary carbonates of cryoarid soils. This observation indicates the soil formation in drained positions under the meadow-steppe vegetation (Sedov et al. 2010). The content of phosphates of various forms in the cultural layers increases significantly. That includes stable apatites that affect the enzymatic activity of soils (Kashirskaya et al. 2017). The transformation of ash into calcium carbonate is also stipulated by physicochemical properties of the cultural layers of “ash coals” typical for the steppe zone and found in the steppes from the Trans-Urals up to Hungary (Kazdym et al. 2003). The composition of clay material changes in both modern and ancient settlement soils. In this context, the cultural layer is considered a type of anthropogenic lithogenesis, and the increased and abnormal concentration of various elements (Pb, Zn, Cu, As, Cd, Ni, Mg) is typical for this kind of soil. Generally, the cultural layer is a zone of anthropogenic processes of sedimentation and diagenesis like natural ones but accelerated. The researchers noted that many minerals might be discovered in cultural layers, even if they are not typical of the background rocks and soils of the region. The authigenic minerals of some cultural layers—carbonates (calcite, aragonite, etc.), sulfate (gypsum, etc.), iron phosphates, calcium phosphates, pyrite, halides (halite)—have already been studied (Kazdym 2001). This conclusion was reached after studying the modern urban soils of Moscow, Smolensk, and St. Petersburg. The following substances have been studied: iron sulfides (pyrite, etc.), sulfate

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(gypsum, jarosite), calcium carbonates (calcite, lublinite, aragonite), and iron carbonates (siderite), iron phosphates (vivianite-boritskite), calcium phosphates (francolite, kurskite, podolite), oxides and hydroxides of iron (goethite, hydrogoethite, lepidocrocite), halides (halite, sylvin), chalcedony in the form of pseudo-morphoses (Kazdym 2001). It is obvious that paleosols from the Bronze Age settlements are less susceptible to such mineral formation; however, the age of 3.5–4 millennia may prevent them from revealing all their features. In any case, paleosols containing cultural layers are unique objects for study. However, the primary goals are to study the fundamental properties of soils of archaeological sites, such as their granulometric composition, and physicochemical properties. The observation of changes in specific properties (for example, the mineral formation), based on their comparison with the background undamaged soils, can be performed only as the second research stage after studying basic properties. For the steppe zone, the share of soil in river valleys impacted by humans in antiquity is about 1% (Plekhanova and Demkin 2005); the traces of such impact are preserved. In this paper, we use the Russian term “paleourbanozems” to label soils containing cultural layers of ancient sites (Plekhanova and Demkin 2005). Simultaneously, the degradation of modern pastures in areas of paleourbanozems is 3–6 times faster. This requires special attention to the composition and properties of paleourbanozems and their integration into modern landscapes of various natural zones.

2 Materials and Methods The study focuses on the materials of the Krasnosamarskoe settlement of the Srubnaya culture (the Timber-grave) of the Late Bronze Age. The data on settlement soils are supplemented by data from three burial mounds of the Poltavka culture of the Krasnosamarskoe-4 burial ground (the Middle Bronze Age). Both sites are located near the village of Krasnosamarskoe in the Samara region of Russia. The archaeological materials of these sites were included in many generalizing works on the origin and migrations of the Eurasia population in the Bronze Age (Haak et al. 2015; Kuznetsov and Mochalov 2017; Vasilyev et al. 2000; Wilkin et al. 2021). Regarding the landscape, the study area is in the southern part of the forest-steppe zone. The climate is continental; precipitation is 400 mm; evaporation is 450 mm; the Selyaninov’s hydrothermal moisture coefficient, taken as a characteristic of the territory moisture supply level, is 0.8–0.9. In geomorphological terms, the sites are located on the second terrace above the floodplain of the Samara River. There, Samara shares the terrace with the valley of the Volga River. The modern soil and vegetation cover are characterized by diversity, and the variability of the microrelief shapes them. Most current forms of microrelief are of water-accumulation and deflationary origin. The polygonality of the soil-ground layer plays a specific role in forming the forms and tortuosity of the watercourses.

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We have conducted morphological descriptions of the 19 soil cross-sections, including six revealing natural soil accumulations, six on the settlement, and seven studying the Poltavka culture burial mounds. Morphological comparisons were made on all 19 sections. In addition, the analysis of physicochemical properties was carried out on the six cross-sections of modern background soils, the two cross-sections of settlement soils, and the four sections through mounds of the kurgans barrows. The samples were processed using various methods to obtain various data. The following methods of soil determination were used: the organic carbon method followed by Tyurin’s method; cation exchange capacity; salt composition of water extract; granulometric soil composition; phosphates by the Machigin’s method conducted photometrically on a UNICO-1200 spectrophotometer, USA, 2012.

3 Results and Discussion The site’s modern soil and vegetation covers are characterized by extreme microdiversity and variability of the microrelief. Chernozem solonetsous soil predominates in the area, showing relics of several cycles of solonetzization. The virgin soils of the site are represented by three major types: meadow-chernozem, solonetzic soils, and alkali, accompanied by intermediate soils, namely, solonetsous meadowchernozems, and saline solonetzic soils.

3.1 The Krasnosamarskoe-4 Cemetery The soils preserved under the Middle Bronze Age kurgans were formed during a relatively humid period. The process of the chernozem formation prevailed over all others, which is clearly expressed by the well-preserved granularity and coproliteness of the upper horizons. The saline solonetzic soils, both in mounds and those inside the modern background soils, were subjected to deflation. Current fluctuations of the meso-microrelief are 30–50 cm. These are the blown-out and degraded areas surrounding meadow communities that remain on micro elevation due to being more degradation-resistant due to the dense vegetation cover.

3.2 The Krasnosamarskoe Settlement The boundaries between the cultural layer and buried soil are visible in all cases inside of “paleourbanosoils.” The lower part of the buried soil is represented by the [A/B] horizon. Its thin tongues-cracks are undoubtedly relics of the continental climate era which occurred before the construction of the settlement, i.e., over 3500 years

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ago. The layer is well preserved at depths of greater than 50 cm. The cultural layers are varied. Dark, light gray, and black cultural layers with different properties and origins result from various anthropogenic activities. The solonetzic structures of two generations, with various sizes of columnar jointing (with cracks and jointings, each is 7–10 cm, and a thin-columnar solonetzic soil with jointings of 3–5 cm in width and up to 5–7 cm in length) have been discovered. Two generations of solonetzic soils in the Krasnosamarskoe settlement were discovered for the first time. The researchers have briefly noted that their characteristics are untypical for soils of the Ural-Volga region (Ivanov et al. 2001). This fact is important for considering the history of saline soil formation. In other sites, they morphologically merge into single layers. Later, the authors described similar solonets structures (the double formation of the solonetzic horizon within the modern cultural layer horizon) n the Bashkir Trans-Urals at the Bronze Age settlements of Novo-Bayramgulovskoye (Rafikova et al. 2017) and the Bronze Age settlement of Ishkininskoe (Plekhanova and Tkachev 2013). There is a correlation between the soil-vegetation cover and the microrelief in the steppe zone: meadow-chernozem soils are formed in the moist depression, whereas less moisture, xeromorphism is typical for microelevations, and a wick saline effect is common for close saline groundwater. However, there is a phenomenon of inversion of vegetation cover and microrelief. As a result, there are reverse relationships: meadow communities on chernozem-meadow soils are located at mesomicroelevations, and wormwood-fescue communities on solonetzic and alkaline soils are located in micro depressions (Plekhanova 2019). Anthropogenic pressure, which caused rapid soil deflation, may explain the observed inversion at the settlement. The modern soil cover is characterized by the predominance of chernozem solonetzic soil complexes with solonetzic soil complexes and relics of several cycles of solonetzization. We consider these inversion ratios as an indicator of the anthropogenic load on the landscape of society in the different eras. The first stage of excessive grazing occurred in the Late Bronze Age (4000–3500 BP) when the above said inverse ratios were established. In other words, the complexity of the soil cover existing today was formed in the Subboreal. Aridization of climate within the period of 2500–2000 BP made it possible to consolidate the established relationships, which even existed at the end of the second millennium CE. Moreover, in the twentieth century, a sharp increase in the anthropogenic load caused rapid cover degradation, so the observed inversions became sharper and observable in the floodplain terraces of the steppe rivers. Because of the conducted paleosol studies, it became clear that the solonetzicchernozem soil complexes have existed in this area for a long time.

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4 Conclusions In the background soils near the Krasnosamarskoe sites, the following two stages of soil development are recorded: 1. The formation of meadow chernozem soil with a humus horizon of up to 75 cm. The meadow-chernozem soil was relatively slightly humic, nonsaline, and was not in balance with the environment since a clear carbonate horizon was not yet formed; 2. The solonetzic soil formed on the meadow soil, while the modern solonetzic soil is inactive and weakly expressed. Before the burial mounds (4800–4200 BP), the soils were free-saline, whereby after mound construction, solonetzic soils periodically formed actively during the last four millennia. Fragmentary buried surfaces of the Srubnaya culture period were discovered at the settlement site. In contrast, the surface of the Srubnaya culture was subsequently subjected to erosion and covered by water sediments. Modern soil-vegetation groups were studied along with paleosols under-mound soils referred to as the Bronze Age. The modern soil cover is characterized by the predominance of saline chernozem solonetsous soil complexes with relics of several salinization cycles. The soils preserved under mounds were formed during a wetter period characterized by prevailing the processes of chernozem formation with wellpreserved granularity and the earthworm dejection structure of the upper horizons. The complexity of the soil cover existing today was formed in the Subboreal (or in the Late Bronze Age), which is 4000–3000 years ago. The age of the mounds used for studying saline solonetzic soils and chernozem-meadow solonetsous soils. During subsequent series of aridizations in the first millennium BCE (in the Iron Age), these inversions were repeatedly fixed and intensified. In all cases, there are anthropogenically transformed soils with various degrees of transformation, and new soil horizons (cultural layers) built into the system of horizons of natural soils. The accumulation of data on the properties of cultural layers will make it possible to describe the diversity of natural and anthropogenic deposits, currently classified as cultural layers. Acknowledgements During participation in excavations carried out by the international archaeological expedition, the Survey Administration (P. F. Kuznetsov, O. I. Mochalov, A. A. Khokhlov, and David W. Anthony) kindly provided us with a possibility to make soil sampling for further analysis of the physical and chemical composition using the assets of the Arkaim reserve (Prof. G. B. Zdanovich, paid travel to the object, meals on the expedition, reagents for chemical analysis), and the resources of the Research Equipment Sharing Center (TsKP) of the Institute of physicochemical and biological problems in soil science under the Pushchino Scientific Center for Biological Research of the Russian Academy of Sciences, the Federal Research Center (Pushchino, the Russian Federation), under the research project, State Assignment No AAAA-A18-118013190175-5.

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References Demkin, V.A., Borisov, A.V., Demkina, T.S., Udaltsov, S.N.: Soil evolution and climate dynamics in the steppes of South-East Russian plain within the Neolith and Bronze Epochs (IV–II MIL. BC). Izvestiya Rossiiskoi Akademii Nauk. Seriya Geograficheskaya 46–57 (2012) (in Russian) Golyeva, A., Khokhlova, O., Lebedeva, M., Shcherbakov, N., Shuteleva, I.: Micromorphological and chemical features of soils as evidence of Bronze Age ancient anthropogenic impact (Late Bronze Age Muradymovo settlement, Ural region, Russia). Geosciences (Switzerland) 8(9), 313 (2018) Ivanov, I.V., Plekhanova, L.N., Chichagova, O.A., Chernyanskiy, S.S., Manakhov, D.V.: Paleopochvy Arkaimskoy doliny i Samarskogo regiona kak indikator ekologicheskikh usloviy v epokhu bronzy (Paleosols of the Arkaim valley and the Samara region as an indicator of ecological conditions in the Bronze Age). In: Bronzovyy vek Vostochnoy Yevropy: kharakteristika kultur, khronologiya i periodizatsiya: Materialy mezhdunar. nauchnoy konferentsii. Samara (Bronze Age of Eastern Europe: Characteristics of Cultures, Chronology and Periodization: Proceedings of the Intern. Scientific Conference), Samara, pp. 375–384 (2001) (in Russian) Haak, W., Lazaridis, I., Patterson, N.: Massive migration from the steppe was a source for IndoEuropean languages in Europe. Nature 522, 207–211 (2015) Kashirskaya, N.N., Plekhanova, L.N., Udaltsov, S.N., Chernysheva, E.V., Borisov, A.V.: The mechanisms and time factor of the enzyme structure of a paleosoil. Biophysics (Russian Federation) 62(6), 1022–1029 (2017) Kashirskaya, N., Chernysheva, E., Plekhanova, L., Borisov, A.: Thermophilic microorganisms as an indicator of soil microbiological contamination in antiquity and at the present time. Int. Multidisc. Sci. GeoConf. Surveying Geol. Min. Ecol. Manag. SGEM 19(3), 569–574 (2019) Kazdym, A.A.: Tekhnogennyye neogeologicheskiye otlozheniya – kulturnyye sloi i protsessy autogennogo mineraloobrazovaniya (Technogenic neogeological deposits—cultural layers and processes of autogenic mineral formation). In: Vestnik Rossiyskogo universiteta druzhby narodov. Seriya: Ekologiya i bezopasnost’ zhiznedeyatelnosti (Bulletin of the Peoples’ Friendship University of Russia. Series: Ecology and Life Safety), vol. 5, pp. 45–53 (2001) (in Russian) Kazdym, A.A., Koryakova, L.N., Kovrigin, A.A., Berseneva, N.A.: Petrograficheskoye i mineralogicheskoye issledovaniye “zol’nikov” Pavlinova gorodishcha (V v. do n. e., Kurganskaya oblast) (Petrographic and mineralogical study of the “ash pans” of Pavlinov settlement (5th century BC, Kurgan region)). Mineralogiya Tekhnogeneza (Mineral. Technogenesis) 4, 198–203. Miass: RAS (2003) (in Russian) Kuznetsov, P., Mochalov, O.: Radiocarbon dating of pottery from bronze age sites in eastern European steppes (Russia). Radiocarbon 59(1), 109–116 (2017) Plekhanova, L.N.: Anthropogenic degradation of soils on river terraces in the Volga-Ural region in the Bronze Age and its effect on the modern soil-plant cover. Arid. Ecosyst. 9(3), 187–192 (2019) Plekhanova, L.N.: Influence of paleoclimatic environment on soil magnetic susceptibility. In: Springer Proceedings in Earth and Environmental Sciences, pp. 20–26 (2021) Plekhanova, L.N., Demkin, V.A.: Ancient soil disturbances in river valleys within the steppe zone of the Southeastern Urals. Eurasian Soil Sci. 38(9), 973–982 (2005) Plekhanova L.N., Tkachev V.V.: Fiziko-khimicheskiye svoystva pochv mnogosloynogo poseleniya epokhi bronzy v okrestnostyakh g. Gay (Physical-chemical properties of the soils at the multilayerd Bronze Age settlement in the surroundings of guy town). Povolzhskaya Arkheologiya 4(6), 225–234 (2013) Plekhanova, L.N., Tupakhina, O.S.: Paleocryogenic traces of climatic peaks of the Late Pleistocene periglacial hyperzone of the mammoth steppe in soils of archaeological sites. IOP Conf. Ser. Earth Environ. Sci. 817(1), 012086 (2021) Rafikova, Ya.V., Fedorov, V.K., Plekhanova, L.N.: Paleopochvennyye osobennosti ritual’nykh ob”yektov i poseleniy bashkirskogo zaural’ya (svyatilishche bakshay) (Paleosol features of ritual objects and settlements of the Bashkir Trans-Urals (Bakshai sanctuary)). In: Borisov, A.V.,

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Plekhanova, L.N., Udaltsov, S.N. (eds.) Paleosols, Paleoecology, Paleoeconomics, pp. 157–162 (2017) Sedov, S.N., Solleiro, E., Khokhlova, O.S., Sinitsyn, A.A., Korkka, M.A., Rusakov, A.V., Ortega, B., Rozanova, M.S., Kuznetsova, A.M., Kazdym, A.A.: Late Pleistocene paleosol sequences as an instrument for the local paleographic reconstruction of the Kostenki 14 key section (Voronezh oblast) as an example. Eurasian Soil Sci. 43(8), 876–892 (2010) Vasilyev, I.B., Kuznetsov, P.F., Turetskiy, M.A., Kuzmina, O.V., Semenova, A.P., Sedova, M.S., Kolev, Yu.N., Kosintsev, P.A., Roslyakova, N.V., Khokhlov, A.A.: Istoriya Camarskogo Povolzhya s drevneyshikh vremen do nashikh dney. Bronzovyy vek (History of the Samara Volga region from ancient times to the present day. Bronze Age), Samara (2000) (in Russian) Wilkin, S., Ventresca Miller, A., Fernandes, R.: Dairying enabled Early Bronze Age Yamnaya steppe expansions. Nature 596, 629–633 (2021)

The Isotopic Signature of Ancient People from the Eneolithic and Bronze Age Interments in the Mountain-Forest Trans-Urals Olga N. Korochkova, Daria V. Kiseleva, Ivan A. Spiridonov, and Evgeny S. Shagalov Abstract The material for the study was provided by two graves excavated in the territory of the Eneolithic (Shaitan 4–6) and the Bronze Age (Shaitan Lake II) archaeological sites. The sites were located on the opposite shores of the Shaitan Lake in the Kirovgrad district of the Sverdlovsk region, Russia (Fig. 1). The abundant grave goods of the Eneolithic burial (the IV–III millennia BCE) included several items that were not typical for the local archaeological context. Additionally, the nearest outcrops of raw materials used to make those items were located far south of the Middle Trans-Urals. The second grave was excavated in the territory of the Bronze Age (the beginning of the 2nd millennium BCE) Seima-Turbino type sacred place named Shaitan Lake II. A comprehensive study of the archaeological artifacts and anthropological remains using various research methods (radiocarbon, anthropological, isotopic, use-wear, etc.) opens up interesting opportunities for historical reconstruction from the long-term perspective. They helped move the proposed cultural genesis, migrations, and contact models into the plane of reality. The isotopic ratios of strontium 87 Sr/86 Sr in the tooth enamel samples from the Eneolithic (0.710093) and the Bronze Age (0.709613) deceased differed from the local natural ratios of bioavailable strontium from the vicinity of the Shaitan Lake (grass has a value of 0.709053, and mollusk shell’s value is 0.708562). The obtained data indicated the probability of the origin of both persons from an area different from the Shaitan Lake environment geochemical background and (or) different underlying rock geological structure. The identified isotopic signals confirmed the proposed hypothesis about the possible migration of these individuals from the steppe region.

O. N. Korochkova (B) · D. V. Kiseleva · I. A. Spiridonov The Ural Federal University, Ekaterinburg, Russia e-mail: [email protected] D. V. Kiseleva · E. S. Shagalov A. N. Zavaritsky Institute of Geology and Geochemistry, UB RAS Ekaterinburg, Ekaterinburg, Russia E. S. Shagalov Ural State Mining University, Ekaterinburg, Russia © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 N. N. Ankusheva et al. (eds.), Geoarchaeology and Archaeological Mineralogy—2021, Springer Proceedings in Earth and Environmental Sciences, https://doi.org/10.1007/978-3-031-16544-3_4

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Keywords Middle Ural · The Eneolithic · The Bronze Age · Interments · Isotopic signature

1 Introduction Until recently, only certain artifacts served as primary evidence, however quite controversial, for the reconstruction of various ancient populations’ mobility models. Simultaneously, the question of whether the non-local cultural evidence or the presence of non-local raw materials resulted from the drift of things or the movement of people has remained unanswered. Though, it would be incorrect to put the question that way. No drift of things would have been possible without the movement of people. It is obvious. The remaining questions are who were the direct participants and the scale of that drift. Who were they, and from what territories had they migrated? Were those exchanges occasional, or were they a part of large-scale migrations? Nowadays, isotopic analysis allows tracing various scenarios of this type of mobility. Strontium isotopes provide information about the movements of people and animals. Isotopes of lead are the source of copper ore raw materials. This type of research technique translates the archaeological hypotheses into the category of verifiable models. However, the researchers dealing with the materials from the mountain-forest Trans-Urals are at a certain disadvantage in this respect. The bone preservation in this environment is extremely poor; hence, the potential for using strontium isotopic signatures for analytical purposes is quite limited. Any possibility of conducting such analysis often relies on a researcher’s pure luck. The sporadic conclusions obtained so far can hardly claim to be definitive, but, in any case, they are undoubtedly interesting and help to test the proposed hypotheses. This study, the isotopic analysis data contributed to interpreting certain specific archaeological situations.

2 Materials and Methods Our attention was focused on two graves excavated on the shore of the Shaitan Lake in the Kirovgrad district of the Sverdlovsk region, Russia (Fig. 1). One of two graves was located in the territory of the Eneolithic settlement (the IV– III millennia BCE) of Shaitan 4–6 on the northeast shore of the lake. The oval-shaped earth grave of 1.6 m × 0.56 m × 0.07 m contained the remains of a male (?) individual of 18–35 years of age. Grave goods consisted of 60 items: three massive knives, 19 arrowheads, 17 flint blades for an insert type tool, 15 clinkstone beads, an adze, a dart, a multifunctional blade tool, and two tablets. The complex stood out in the presence of objects of apparently “southern” origin, namely, the brown siliceous schist knives (Fig. 2a). The nearest known outcrops of this type of raw material were located in the territory of northern Kazakhstan and the southern Urals. Analogies to the massive

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Fig. 1 Archaeological sites of Shaitanskoe Ozero II, Shaitanskoe Ozero 4–6 on the map of Eurasia

knife could be found in the materials of the North Kazakhstan Botai culture (Zaibert 2011, Fig. 2), the Eneolithic Altai complexes (Kiryushin 2002, Fig. 31, 32), and the Khvalyn culture of the steppe Cis-Urals (Morgunova 2011, Fig. 64). Another grave was excavated in the territory of the Seima-Turbino type sacred place Shaitan Lake II on the western shore of the lake. The grave was placed among other interments at the sacred place on the western periphery (Korochkova et al. 2020, p. 44–47). The shallow pit had a rectangular shape and measured 1.8 m × 0.7 m × 01 m. It contained cremated remains of a 25–30 years-old female individual. The radiocarbon analysis of coal from the burial produced the following results: 3575 ± 30 BP (Poz–71112); 3575 ± 29 BP (MAMS–23961) (Chernykh et al. 2017). Preserved fragments of a bracelet with a spiral ending were found in the area of the right arm (Fig. 2b). Similar bracelets were a typical female costume accessory of the Petrovka-Alakul cultures of the southern Urals and northern Kazakhstan. Many signs related to those archaeological cultures symbolized the sacred place (Korochkova and Spiridonov 2021). This symbol indicates the steppe impulse in forming the phenomenon of the first metallurgists of the Middle Urals, who built the

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Fig. 2 a Shaitanskoe Ozero 4–6, the Eneolithic complex; b Shaitanskoe Ozero II, the Bronze Age complex

Shaitan Lake II sacred place. In this regard, it is particularly interesting to discover the origins of a woman from burial 8. The scarce anthropological remains from those graves contained tooth enamel fragments suitable for isotopic analysis. Vegetation and mollusk shells from Shaitan Lake were used as natural local samples.

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The sample preparation and measurements were carried out in a cleanroom (6, 7 ISO) of the Institute of Geology and Geochemistry UB RAS, Ekaterinburg. Ultrapure deionized water (18.2 M .·cm−1 ) was used at all stages of the analysis. All the labware and materials contacting the reagents and samples were made PFA (Savillex), PTFE (Nalgene) or polypropylene (Sarstedt). All used acids were purified twice by sub-boiling distillation (Savillex, USA; Berghof, Germany). Bioavailable Sr proxies (plants and mollusk shells) and two samples of human enamel were pre-cleaned and dissolved, and Sr was chromatographically separated according to the protocols described in Kiseleva et al. (2021). The Sr isotope composition was determined using a Neptune Plus (Thermo Fischer) double-focusing multi-collector magnetic sector mass spectrometer by the SSB bracketing technique with the NIST SRM 987 Sr carbonate isotope standard. To assess the accuracy and long-term reproducibility of the measurement procedure, NIST SRM 987 was used: 87Sr/86Sr = 0.710266 ± 8 (1SD, N = 23).

3 Results and Discussion The Eneolithic burial stands out against the background of the known Eneolithic interments of the mountain-forest Trans-Urals by the presence of tools that were quite untypical for the local archaeological context. No examples of this type of raw material were found among the numerous lithic waste items. These facts suggest a hypothesis of the “southern” origin of the buried person and are further tested using the isotopic analysis technique. The set of massive knives is unusual for the local Eneolithic culture (Fig. 2a, 21). They made are of siliceous schist, the known outcrops of which were located in the southern Ural and northern Kazakhstan. The knives point to the steppe belt cultures as the source of origin. Another indication of the possible connection with the Andronov community steppe cultures was the only artifact from the Bronze Age burial. The obtained isotopic analysis results confirmed the hypotheses of the possible migration of the deceased individuals. The isotopic ratios of strontium 87 Sr/86 Sr in enamel samples from the excavations of 2021 (0.710093) and 2013 (0.709613) were highly radiogenic. They differed from the background ratios of bioavailable strontium from the vicinity of Shaitan Lake: grass taken from the immediate vicinity of the excavation site measures 0.709053, and a mollusk shell has a value of 0.708562. The obtained data indicated the probability of the origin of both persons from an area different from the Shaitan Lake environment geochemical background and (or) different underlying rock geological structure. According to the published data on the distribution of strontium isotope ratios in watercourses and reservoirs in the southern part of the Chelyabinsk region (Epimakhov et al. 2021), the maximal radiogenic values of 87 Sr/86 Sr lie within the range of 0.70985–0.71588, and geologically correspond to the East Ural structuralformation megazone. Similar strongly radiogenic isotope ratios of 87 Sr/86 Sr (0.7095– 0.7100) are also typical for the watercourses of the Svetlinsky district of the Orenburg region bordering Kazakhstan. Nevertheless, we should not exclude from the list of

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places of the possible origin of those individuals from the Middle Urals locations in the granite belt area (e.g., the Murzinsky-Aduysky gneiss-granite complex), which, due to the underlying rocks with radiogenic strontium values from 0.704 to 0.735 (Montero et al. 2000), can also produce high background ratios of 87 Sr/86 Sr bioavailable strontium. The measured ratios in the granitoid of the Upper Iset batholith, within which both the lake and site are located, vary from 0.704 to 0.709 (Fershtater et al. 2019) and, with a high degree of probability, cannot produce higher values of bioavailable strontium. The presence of the untypical archaeological artifacts along with the isotopic analysis of human tooth enamel data may, with a certain degree of probability, indicate the origin of the buried individuals from the steppe regions of the Southern Urals bordering northern Kazakhstan.

4 Conclusions A comprehensive study of the archaeological artifacts and anthropological remains using various research methods opens up interesting opportunities for historical reconstruction from a long-term historical perspective and moves the proposed cultural genesis, migration, and contact models into the plane of reality. The Eneolithic burial at Shaitan 4–6 settlement was interpreted as the autonomous burial of a male individual—an immigrant from the steppe region. The female burial in the territory of the metallurgists’ sacred place, Shaitan Lake II may be interpreted as a manifestation of the special status of the representative of the local metallurgist clan closely related to the steppe region. Acknowledgements The article was prepared within RFBR project no. 21-78-20015 «Technologies of mining and metallurgical production of the Bronze Age in the evolution of the culturalhistorical landscape of the Ural region», as well as within the state assignment of the Ministry of Science and Higher Education of the Russian Federation, theme: “Regional Identity of Russia: Comparative Historical and Philological Studies,” topic no. FEUZ-2020. Sr isotopic analyses were supported by the Russian Foundation for Basic Research (project no. 20-09-00194) and performed at the “Geoanalitik” shared research facilities of the IGG UB RAS. The re-equipment and comprehensive development of the “Geoanalitik” shared research facilities of the IGG UB RAS was financially supported by a grant from the Ministry of Science and Higher Education of the Russian Federation (Agreement No. 075-15-2021-680).

References Chernykh, E.N., Korochkova, O.N., Orlovskaya, L.B.: Issues in the calendar chronology of the Seima-Turbino Transcultural Phenomenon. Archaeol. Ethnol. Anthropol. Eurasia 45(2), 45–55 (2017) Epimakhov, A.V., Ankushev, M.N., Ankusheva, P.S., Kiseleva, D.V., Chechushkov, I.V.: Predvaritelnye rezultaty analiza izotopov strontsiya v ramkakh izucheniya mobil’nosti naseleniya

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bronzovogo veka Zauralya (Preliminary results of the strontium isotopes analysis in the framework of the study of the mobility of the Bronze Age population in the Trans-Urals). Geoarkheologiya i Arkheologicheskaya Mineralogiya (Geoarchaeology and Archaeological Mineralogy) 8, 11–17 (2021). (in Russian) Fershtater, G.B., Krasnobaev, A.A., Montero, P., Bea, F., Borodina, N.S., Vishnyakova, M.D., Soloshenko, N.G., Streletskaya, M.V.: Vozrastnye i izotopno-geohimicheskie osobennosti murzinsko–adujskogo metamorficheskogo kompleksa v svyazi s problemoj formirovaniya Murzinskogo mezhformacionnogo granitnogo plutona (Age and isotope-geochemical features of the Murzinka-Adui metamorphic complex in connection with the problem of formation of the murzinka interformational granite pluton). Rossijskaya geologiya i geofizika (Russian Geology and Geophysics) 60(3), 287–308 (2019) (in Russian) Kiseleva, D.V., Ankusheva, P.S., Ankushev, M.N., Okuneva, T.G., Shagalov, E.S., Kasyanova, A.V.: Opredelenie fonovyh izotopnyh otnoshenij biodostupnogo stronciya dlya rudnika bronzovogo veka Novotemirskij (Bioavailable strontium isotope baseline for the Novotemirskiy Bronze Age mine). Kratkiye Soobshcheniya Instituta Arkheologii (Brief Communications of the Institute of Archaeology) 263, 176–187 (2021). (In Russian) Kiryushin, Yu.F.: Eneolit i rannyaya bronza yuga Zapadnoj Sibiri (The Eneolithic and Early Bronze Age of the South of Western Siberia), p. 294. Izdatelstvo Altajskogo universiteta, Barnaul (2002) (in Russian) Korochkova, O.N., Stefanov, V.I., Spiridonov, I.A.: Sviatilishche pervykh metallurgov Urala (Sacral Place of the first metallurgists of the Urals), p. 214. Izdatelstvo Uralskogo universiteta, Ekaterinburg (2020) (in Russian) Korochkova, O.N., Spiridonov, I.A.: Novye nakhodki kremnevoj plastiki v gorno-lesnom Zaural’e (New finds of flint plastic art in the Mountainous-Forest Trans-Urals). Kratkiye Soobshcheniya Instituta Arkheologii (Brief Communications of the Institute of Archaeology) 264, 193–200 (2021). (in Russian) Montero, P., Bea, F., Fershtater, G., Zinkova E.: Single-zircon evaporation ages and Rb-Sr dating of four major Variscan batholiths of the Urals. A perspective on the timing of deformation and granite generation. Tectonophysics 317, 93–108 (2000) Morgunova, N.L.: Eneolit Volzhsko-Uralskogo mezhdurech’ya (The Eneolite of the Volga-Ural interfluve), p. 220. Izdatelstvo Orenburgskogo universiteta, Orenburg: OGPU (2011) (in Russian) Zaibert, V.F.: Botaj. U istokov stepnoj tsivilizatsii (Botaj. At the origins of the steppe civilization), p. 480. Balausa, Almaty (2011) (in Russian)

Results of Geochemical Research at the Suursuonmäki Early Iron Age Burial Mound Mikhail A. Streltcov, Marianna A. Kulkova, and Maria A. Razzak

Abstract This article presents the results of geochemical studies at the Suursuonmäki burial mound. Using an XRF research method, data on the chemical composition of 40 soil samples from 2 sites of the monument were obtained. The anthropogenic activities of ancient people can significantly influence the chemical composition of soils, enriching or exhausting some elements. The method of reconstruction of functional zones by using geochemical indicators made it possible to reveal a correlation between the values of changes in anthropogenic activity and indicators that characterize traces of bone, charcoal remains, and wood ash. Keywords Geochemical indication · Archaeology · Outer islands of Gulf of Finland · Early Iron Age · Burial mound

1 Introduction The Suursuonmäki burial ground is located in the Outer Islands of the Gulf of Finland. The history of their archaeological investigation comprises two periods. The first was during the pre-war period when the islands were part of Finland. During those years, information from residents about particular archaeological sites and finds from the islands had been accumulated, and professional archaeological excavations and surveys were carried out. Then, during the second half of the twentieth century, the islands were not available for the scientific study being a border zone of the USSR. In the past 20 years, a new period of field research has begun, but the results are not published. In 2019, the IIMK RAS expedition conducted archaeological exploration under the leadership of M.A. Razzak, the main work was carried out on Moshchny M. A. Streltcov (B) · M. A. Kulkova Herzen State Pedagogical University, Saint-Petersburg, Russia e-mail: [email protected] M. A. Razzak Institute for the History of Material Culture, Russian Academy of Science (IIMK RAS), Saint-Petersburg, Russia © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 N. N. Ankusheva et al. (eds.), Geoarchaeology and Archaeological Mineralogy—2021, Springer Proceedings in Earth and Environmental Sciences, https://doi.org/10.1007/978-3-031-16544-3_5

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Fig. 1 Islands of the Gulf of Finland where the archaeological surveys of 2019 were conducted. In circle—Island Moshchny (Lavansaari)

island (Lavansaari) (Fig. 1). Several Bronze Age–Modern Age archaeological sites have been surveyed and identified (Razzak 2021). The Quaternary deposits of this region are represented by sands, varved clays and silt of glaciolacustrine deposits of the second Baltic glacial lake (Apuhtin 1969). The Early Iron Age burial ground Suursuonmäki is located in the western part of Moshchny Island, in the forest, on a low (about 4 m) ridge. Visual inspection revealed 23 mounds with a diameter of 1.5–6 m and a height of up to 0.5 m (Razzak 2021). The mounds are made of stones covered with turf. The shape of the mounds is round or oval, and the tops of most mounds are flattened. Generally, the size of the burial ground is about 110 m long and a maximum of 12 m wide. The distance between the burial mounds ranged from 0.5 to 6 m (Fig. 2). The first information about the monument was received from locals in 1926. At that time, the island belonged to Finland. In 1930, Pälsi carried out work on the burial ground. He has planned the burial ground, where 28 mounds have been marked, and three mounds have been excavated. Human calcined bones, ash, charcoal, and resin pieces have been found. In 1993, Edgren described in detail and examined the results of these excavations (Edgren 1993). Three radiocarbon dates were obtained from the excavation of Pälsi, which, after calibration, indicate the last centuries BC—the first

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Fig. 2 Topographic plan of the cemetery of Suursuonmäki (2019)

century AD: 1975 ± 70 BP (Ua-2545), 1960 ± 70 BPs (Ua-2546), 2165 ± 60 BP (Ua-2547). Monuments of the Early Iron Age in the St. Petersburg region are practically unknown. An only exception is a group of burial grounds with stone enclosures of the Roman period in the south of the Gulf of Finland, discovered only recently (Yushkova 2016). Such burial grounds are called “the tarand graves,” also common in Estonia and Latvia. Suursuonmäki burial ground belongs to another type of monument in terms of structure; it is close to the burial mounds of southeastern Finland. The closest analogy is the Pyhtää Strukankalliot burial ground in the district of Kotka, stone mounds with artifacts of the early Roman period were discovered there (Miettinen 1997). During explorational works at the Suursuonmäki burial ground, samples were taken for the study of functional zones by geochemical research method; the following geochemical indicators were used: P2 O5(anthr) is a geochemical indicator used to characterize the anthropogenic activity on the territory (P2 O5(anthr) = P2 O5 /(P2 O5 + Na2 O)) (Kulkova 2012; Holliday and Gartner 2007). Phosphorus is an inactive chemical element and has low mobility in soil. Compounds of phosphorus are insoluble and resistant to oxidation, reduction, and leaching (Holliday and Gartner 2007). Phosphorus is a major of many organic compounds. It is presented in products that are used on the farm, and phosphorous concentration in the soil increases due to human activity (Kulkova et al. 2015; Schlezinger and Howes 2000; Terry et al. 2000). A correlation has been noted between the increase in the content of heavy metals in soils and the anthropogenic activity of ancient populations (Wilson et al. 2008).

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CaO is the main component of bone tissue, teeth, and horn formation and indicates animal remains and burials. Sr replaces CaO in the process of burial of bones, teeth and horn formation. On the one hand, areas of increased concentrations of these elements are often associated with cutting areas of animals. On the other hand, they are associated with burial sites. K2 O, Rb are elements that are part of charred wood, and ash is an indicator of the hearth zone (Kulkova 2012). High concentrations of Fe2 O3 , MnO2 can be considered as the elements of red (hematite, cinnabar), yellow (ocher), and black (pyrolusite) coloring pigments, which may indicate ritual practice (Wells et al. 2000). Changes in the concentration of silica (SiO2 ) in sediments can be used to reconstruct the microrelief of the site. Sand formations with high quartz content are confined to elevated areas. Clay deposits with a predominance of such chemical elements as Al2 O3 , MgO, CaO, Fe2 O3 , mark depressions in the microrelief. Also, for reconstructing the microrelief, the ratio of the main rock-forming elements is related to sandy and clay deposits SiO2 /(Al2 O3 + MgO + CaO + Fe2 O3 ) have been used (Kulkova 2012). The separation of the chemical elements that marker anthropogenic activity from the components of rock-forming minerals has been conducted using the following ratios: P2 O5(anthr) = P2 O5 /(P2 O5 + Na2 O); CaO(anthr) = CaO/(CaO + Na2 O); K2 O(anthr) = K2 O/(K2 O + Na2 O); Rb(anthr) = Rb/(Rb + Na2 O); Sr(anthr) = Sr/(Sr + Na2 O) (Kulkova 2012).

2 Materials and Methods Forty soil samples were taken from the subsoil without destruction of archaeological objects and excavation to reconstruct the functional zones of the site. Samples № 1–15 have been taken around mound № 2, located in the eastern part of the burial ground. Samples №16–40 have been taken in the western part of the burial ground near mounds № 10, 11, 13–15. Each sample has been packed in a separate sealed bag to avoid mixing samples and, as a result, obtaining unreliable data. Sample preparation has been carried out under laboratory conditions. First, samples were dried in an air-dry condition at t° = 105 °C. Then, 15–25 g samples were ground to powder (particle size < 0.01 mm). Further, in the form of boric acid, the powder was pressed under a pressure of 60–160 bars. Obtained samples were analyzed by the X-ray fluorescence research method (XRF) in «Spectroscan MAX−GV.» The mapping of the distribution of geochemical indicators associated with anthropogenic activity was carried out using the kriging interpolation method in the computer program Surfer 9 (Figs. 3 and 4). Because of vital activity, a person affects the chemical composition of the soil. The preservation of such traces depends on many external factors, such as climate, lithology, and the intensity of anthropogenic activity. However, using geochemical

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Fig. 3 Maps of the distribution of geochemical indicators at the first site—1. Ba(anthr) , 2. CaO(anthr) , 3. Fe2 O3 , 4. K2 O(anthr) , 5. Rb(anthr) , 6. SiO2 , 7. P2 O5(anthr) , 8. Sr(anthr)

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Fig. 4 Maps of the distribution of geochemical indicators at the second site: 1. Ba(anthr) , 2. CaO(anthr) , 3. Fe2 O3 , 4. K2 O(anthr) 5. Rb(anthr) , 6. SiO2 , 7. P2 O5(anthr) , 8. Sr(anthr)

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research methods, these traces of early human activity may still be identified (Oonk et al. 2009). Using a single chemical element or geochemical indicator to characterize an archaeological object may not always be correct in the geochemical reconstruction of functional zones of settlements and burial sites. This is due to the different natural and anthropogenic factors that influence the behavior of chemical elements. Therefore, there is a necessity to use “multi-element” analysis, which allows using a set of elements and geochemical indicators that reflect different functional zones of an archaeological site (Kulkova et al. 2015; Kulkova 2012; Holliday and Gartner 2007; Middlenton and Price 1996; Wilson et al. 2008; Schlezinger and Howes 2000).

3 Results and Discussion The first site is located in the eastern part of the burial mound and lies on the area of stone structure № 2 and partially № 1 (Fig. 3). Analysis of anthropogenic activity in terms of P2 O5(anthr) showed increased values of this indicator near stone structure №2 at sampling points №№ 1, 7, 8, 10, 11, which correlates with the elevation in reconstructed microrelief in terms of SiO2 . Geochemical indicators of bone tissue remnants Sr(anthr) , CaO(anthr) spatially intersect with indicators of anthropogenic activity P2 O5(anthr) , Ba(anthr) and indicators K2 O(anthr) , Rb(anthr) , which show zones associated with the increase in charcoal residues in sediments. Sampling points №14 and №15 were used as background values. The second site occupies the western part, where the stone structures are located closer to each other and lie on the area of stone structures №№ 11, 12, 13, and partially 10, 14, 15 (Fig. 4). Analysis of the indicator of anthropogenic activity P2 O5(anthr) has shown an increase in anthropogenic activity within the area of distribution of stone structures. An anomalous zone with the highest concentration of indicator P2 O5(anthr) is located in the area of samples numbered 16–18, 30–33 and occupies the inner part between stone structures №13 and partially № 11. The zone also intersects with the elevation in reconstructed microrelief in terms of SiO2 and an increase in the concentration of Fe2 O3 , Ba(anthr) . Anomalous zones of geochemical indicators associated with the remnants of bone tissue Sr(anthr) , CaO(anthr) have also been noted. There is a clear correlation between the data of geochemical indicators Sr(anthr) , CaO(anthr), and the indicator of anthropogenic activity P2 O5(anthr) . Analysis of indicators K2 O(anthr) , Rb(anthr) shows the zones of anomalous concentrations, which may be associated with a hearth zone or an increase in charcoal residues in sediments. Increased concentrations of these geochemical indicators are noted in the inner part between the stone structures and towards north from mounds № 15 and 12. A specific anomalous zone has been observed on the stone structure № 12. In the area of this structure, low values of all used geochemical indicators have been found. Sampling point №35 was used as background values.

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The analysis of the obtained geochemical data from the Suursuonmäki site has made it possible to identify the connection between the change values in the anthropogenic activity indicator and geochemical indicators that characterize traces of bone tissue, charcoal residues, and wood ash, which may correspond to the burial ground and may suggest the ritual of body cremation.

4 Conclusions According to geochemical studies, the archaeological site Suursuonmäki may be interpreted as a burial ground. A few archaeological artifacts and previous archeological studies support this interpretation (Miettinen 1996, Razzak 2021). The anomalous zones of geochemical indicators that determine the burial have been obtained via the increased concentration of the combination of such indicators as P2 O5(anthr) , CaO(anthr) , Sr(anthr) , Ba(anthr) , Fe2 O5 . An increase in the remains of charcoal and ash elements is marked by the rise in the concentration of geochemical indicators K2 O(anthr) and Rb(anthr) , which may suggest cremation. Reconstruction of the microrelief at the archaeological site Suursuonmäki, using the study of the geochemistry of the main rock-forming elements, made it possible to establish that the stone formations are located at local elevations. The study of archaeological sites by the method of geochemical indication makes it possible to reconstruct the functional features of sites even with few archaeological artifacts or their absence at all. Also, it is possible to use the geochemical research method without destroying the integrity of such archaeological site as a burial mound. Acknowledgements The reported study was funded by RFBR, project 20-35-90015.

References Apuhtin, N.I.: Geologicheskaya karta chetvertichnyh otlozhenij Leningradskoj, Pskovskoj i Novgorodskoj oblastej (Geological map of Quaternary deposits of the Leningrad, Pskov and Novgorod regions). «Geologiya SSSR» (1969) (in Russian) Edgren, T.: Lavansaaren Suursuonmäen röykkiöhaudat (The mounds of Suursuonmäki in Lavansaari). Suomen Museo 5–20 (1993) (in Finnish) Holliday, V.T., Gartner, V.G.: Methods of soil P analysis in archaeology. J. Archaeol. Sci. 34, 301–333 (2007) Kulkova, M.A.: Metody prikladnyh paleolandshaftnyh geohimicheskih issledovanij (Applied paleolandscape geochemical research methods). Saint-Petersburg (2012) (in Russian) Kulkova, M.A., Gusencova, T.M., Madyanova, N.P.: Primenenie metoda geohimicheskoj indikacii dlya rekonstrukcii funkcional’nyh zon na pamyatnikah kamennogo veka Prinevskogo regiona (Application of the Geochemical Indication Method for the Reconstruction of Functional Zones at the Stone Age Sites of the Prineva Region). Izvestiya Rossijskogo gosudarstvennogo pedagogicheskogo universiteta im. A. I. Gercena № 176, 76–89 (2015) (in Russian)

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Miettinen, T.: Suomenlahden ulkosaarten esihistoria. In Suomenlahden ulkosaaret – Lavansaari, Seiskari, Suursaari, Tytärsaari (Prehistory of the outer islands of the Gulf of Finland. In the outer islands of the Gulf of Finland – Lavansaari, Seiskari, Suursaari, Tytärsaari). Helsinki, pp. 52–67. (1996) Miettinen, T.: The changing picture of the iron age on the northern coast of the eastern part of the Gulf of Finland. Slavs and Finno-Ugrians. Archaeology, History, Culture. In: Reports of the Russian-Finnish Symposium on Archaeology. Saint-Petersburg, pp. 62–70. (1997) (in Russian) Middlenton, W.D., Price, T.D.: Identification of activity areas by multi-element characterization of sediments from modern and archaeological house floors using inductively coupled plasma-atomic emission spectroscopy. J. Archaeol. Sci. 23, 673–687 (1996) Oonk, S., Slomp, C.P., Huisman, D.J.: Geochemistry as an aid in archaeological prospection and site interpretation: current issues and research directions. Archaeol. Prospect. 16, 35–51 (2009) Razzak, M.A.: Archaeological survey of the outer islands of the Gulf of Finland in 2019. In: Materiality and Objects: Multi-disciplinary Approaches to Archaeological Material and Contexts. IKOS 24, pp. 102–113. (2021) Schlezinger, D.R., Howes, B.L.: Organic phosphorus and elemental ratios as indicators of prehistoric human occupation. J. Archaeol. Sci. 27, 479–492 (2000) Terry, R.E., Hardin, P.J., Houston, S.D.: Quantitative phosphorus measurement: A field test procedure for archaeological site analysis at Piedras Negras Guatemala. Geoarchaeol. an Int. J. 15, 151–166 (2000) Wells, E.C., Terry, R.E., Parnell, J.J., Houston, S.D.: Chemical analyses of ancient a thro sols in residential areas at Pieda Negras Guatemala. J. Archaeol. Sci. 27, 449–462 (2000) Wilson, C.A., Davidson, D.A., Cresser, M.S.: Multi-element soil analysis: an assessment of its potential as an aid to archaeological interpretation. J. Archaeol. Sci. 35, 412–424 (2008) Yushkova, M.A.: New group of sites of the 1st to 7th centuries AD in the south-west of Leningrad Oblast. In: New Sites, New Methods The 14th Finnish-Russian Archaeological Symposium. ISKOS 21. Helsinki, pp. 135–151. (2016)

The Use of Rocks and Minerals by Ancient Societies

Mineral Resources of the Jasper Belt of the Southern Urals and Geoarchaeological Objects Peter V. Kazakov

Abstract We analyzed the confinement of deposits of Fe-Mn ores of the West Magnitogorsk ore zone, the occurrences in the Yarlykapov gold ore zone, and the actual deposits of jasper in the Jasper Belt of the Southern Urals and siliceous horizons of volcanogenic-sedimentary strata of the Middle Devonian. According to archival data, the ore deposits of the Jasper Belt have been developed since the 18th century CE. The examples of the earliest human use of jasper-like siliceous schists are dated back to the Stone Age. Keywords Geoarchaeology · Silicites · Jasper · Manganese · Iron · Gold · Deposit · Stone age · Jasper belt · Southern urals

1 Introduction The area is located on the eastern slope of the Southern Urals. It belongs to the Uchalin, Abzelilov, and Baimak districts of the Republic of Bashkortostan, Russia (Fig. 1). The central part of the so-called “Jasper Belt” territory is represented by the most pronounced Kryktytau and Irendyk ridges. The absolute height of individual peaks of the ridges reaches 978 masl and 1118 masl. They rise above the lake chain, located east in the Kizilo-Urtazim depression, by more than 500–600 m. The Kryktytau and Irendyk ridges comprise the Lower, Middle, and Upper Devonian volcanic and volcanic-sedimentary strata. In them, among lava flows, tuff breccias, and tuffs of predominantly basaltic and basaltic andesite composition, there are numerous ridged outcrops of silicites resistant to weathering in the form of lenses, intermittent interlayers, and whole horizons (Yarlykapov) with a thickness of 5–10 to 60–200 m.

P. V. Kazakov (B) Institute of Geology of the Ufa Federal Research Centre RAS, Ufa, Russia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 N. N. Ankusheva et al. (eds.), Geoarchaeology and Archaeological Mineralogy—2021, Springer Proceedings in Earth and Environmental Sciences, https://doi.org/10.1007/978-3-031-16544-3_6

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Fig. 1 The layout of the Fe-Mn deposits of the manganese ore zone of the Magnitogorsk megasynclinorium western side (based on the archival materials of Garris et al. 2002, modified): 1—administrative borders of the Republic of Bashkortostan; 2—railways; 3—centers of administrative districts; 4–5—deposits and occurrences of ferromanganese ores; 6—border of the West Magnitogorsk ore region (A); 7—ore fields of manganese deposits

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On the southern closure of the Irendyk ridge and its southeastern spurs, the Baishevsky archaeological district (AMD) is located. About two hundred settlement, burial, and industrial archaeological sites dating from the Stone Age to the Late Middle Ages and historic times have been identified within its borders (Gusev et al. 2010). The main research objects are the ore and nonmetallic minerals of the jasper belt. The tasks are as follows: (1) to identify the conditions for the formation of silicites and localization of ferromanganese ores and gold deposits, (2) to examine the features of the material composition of ores, and (3) the depletion of deposits and the possibility of involving them in further exploitation.

2 Materials and Methods From 1998 to 2005, the team of researchers from BashGeolCenter, Ltd, including the author, conducted a geological and economic assessment of ore (Mn, Au) and placer (Au) deposits in the Republic of Bashkortostan. The methodology of the work consisted of: (1) collection, study, and generalization of archival and published materials of geological exploration and operational work; (2) resource assessment of manganese and gold deposits; (3) recommendations for further exploration and operational work (4) the study of deposits as objects of geoarchaeology, the possible use of minerals of the jasper belt by ancient man.

3 Results and Discussion The silicites of the Yarlikapov horizon are presented by thin-, medium- and thicklamellar, less often massive jasper-like siliceous schists, dark gray, black (lidites, phtanites), less often light bluish-gray; red-green jasper, and iron-siliceous jasper tuffites. Rocks have a characteristic conchoidal fracture with cutting edges. A quartz composition and micro-grained structure represent jasper. Jasperoids are predominantly represented by chalcedony (cryptocrystalline fine-fibrous type of quartz) composition. In jasper flints and jaspers, radiolarians and conodonts are inhabitants of the Devonian seas with a silicon skeleton. The ferromanganese deposits of the manganese ore zone of the western flank of the Magnitogorsk megasynclinorium (see Fig. 1) are associated with hydrothermalhydrogenous enrichment of silicites of the Yarlikapov horizon with Mn and Fe. It extends in the meridional direction from the environs of the city of Miass in the north to the latitude of the village of Buribay in the south (Salikhov et al. 2002, p. 39). The rich ores of the deposits are localized in “iron-manganese hats” and owe their origin to the processes of hypergenesis with the appearance of semi-oxidized and oxidized ores. The hypergenesis depth distribution reaches 35–60 m, rarely—200– 280 m. Secondary oxide ores are characterized by the Mn content of 35–40 %, the

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Fe content of up to 10–28 %, and the SiO2 content of up to 5–35 %. In primary ores, the silica content reaches 56 %, limiting their metallurgy use. With brecciated intensely hydrothermally processed jasperoids of the Yarlykapovsky horizon are associated with small deposits of gold in the Yarlykapov gold ore zone, which stretches for more than 50 km along the eastern slope of the Irendyk ridge (Menshikov et al. 1997). Mineralization in them is represented by disseminated dissemination of pyrite (FeS) in silicified siliceous schists and jaspers. In some deposits, the total thickness of the sulfidized jasper zone reaches 15–20 m, and the length is 60–200 m. The average gold content in mineralized jaspers does not exceed 3–4 ppm, in some areas with massive vein silicification exceeding 10–15 ppm. Gold in ores is coarse in native form and finely dispersed in pyrite (FeS). The gold sample is 800–900. The horizons of mineralized jasper are one of the sources of placer gold in the East-Irendyk zone. All the manganese and gold deposits of the western flank of the Magnitogorsk megasynclinorium associated with jasperoids were discovered at the end of the 18th—first third of the 20th centuries CE, and many of them were brought into production (Humboldt 1830; Betechtin 1940). There is no earlier information about mining in the archives. The deposits were characterized by the high quality of mined ores and favorable mining conditions. They were mined before the depletion or complete excavation of the near-surface bodies of rich oxide ores, and only in some cases was mining carried out at depths of more than 20 m. In the eastern part of the jasper belt of the Southern Urals, at the foot of the Kryktytau and Irendyk ridges, there is a garland of lakes: Ulyandy, Karabalykty, Sabakty, Yakty-Kul (Bannoe), Surtandy, Chebarkul, and Koltuban (from north to south). Deposits of decorative and ornamental jasper with the same name are known there. The history of the search for jasper and the appearance of the first quarries in the Urals dates back to the 17th century AD. The South Ural jasper was used in the architectural and sculptural decoration of the rooms of the Winter Palace, the State Hermitage, the imperial chambers in St. Petersburg, in Tsarskoye Selo, when many Bashkir jaspers were already known for their magnificence: Kushkuldinskaya Tungatarovskaya, Beloagatinskaya, Tashbulatovskaya, Urazovskaya, and Kalkan. According to Fersman, the first Jasper stones, which began to be polished at the Peterhof lapidary mill, were Bashkir jasper (Fersman 1954, p. 161). Currently, only within the Republic of Bashkortostan, more than 200 deposits and occurrences of jasper are known (Salikhov et al. 2012) (Fig. 2). But the earliest use of jasper-like siliceous schists and jaspers dates back to the Stone Age, the longest period in human history. In the north rim of the KiziloUrtazym depression, on the western shore of the lake Karabalykty, the Urals’ oldest Upper Paleolithic site the Mysovaya (Urta-Tyube) Campsite—was found (Bader and Matyushin 1973; Matyushin 1973). The site is a multi-layered settlement of the Acheulean-Mousterian culture. The materials of the Paleolithic layer of this site consist of Acheulean-type sharp points, scrapers, and choppers made of dark gray jasper. One of them is made on the end of an oval jasper pebble. The inventory of the Mesolithic layer is represented by numerous incisors of lance-shaped plates of various shapes. Among them are double

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Fig. 2 Geological scheme of deposits and occurrences of jasper in the central part of the Jasper Belt of the Southern Urals (according to Salikhov et al. (2012), modified): 1–12— multitemporal structural-material complexes (1–3—Riphean; 4—Ordovician; 5—Silurian; 6— Devonian; 7—Lower Middle Devonian (Irendyk); 8–9—Middle Devonian (Bugulygyr, Karamalytash); 10—Middle-Upper Devonian (Ulutau); 11—Upper Devonian (Zilairian); 12—coal); 13—Neogene and Quaternary deposits; 14–16—intrusive formations: 14—granites; 15—gabbrodolerites; 16—ultramafic; 17—deposits and occurrences of jasper, their numbers (1—Bayramgulovo; 2—Kushkuldino (Nauruzovo); 3—West-Nauruzovo; 4—Abzakovo; 5—Gabdimovo; 6— Niyazgulovo; 7—Ulyandykul; 8—Tashbulatovo; 9—Karabalyktino; 10—Sabaktino; 11—Kusimovo (Lake Bannoe); 12—Alimbetovo; 13—Kucharovo; 14—Kusheevo; 15—Askarovo; 16— West-Askarovo; 17—Chebarkul; 18—Idyash; 19—Yuzhno-Kulukasovo; 20—Beloagatinsky; 21— Yuldashevo; 22—Ursuktamak; 23—Aktau; 24—Angala; 25—Gubaidullino; 26—Tubinsky; 27— Talkass; 28—Isyanovo; 29—Bakhtigareevo; 30—Serekkul; 31—Mryasovo; 32—Kuliurtau; 33— Asylovo; 34—Turkmenevo; 35—Severnaya Sopka; 36—Bugulygyr; 37—Zapadno-Davletovo; 38—Davletovo; 39—Karjukmas; 40—Karagailino; 41—Sibai; 42—Karamalytash; 43—Aisuak; 44—Starosibay; 45—Yumashtau; 46—Yuzhno-Khasanovo; 47—Khasanovo; 48—Kuskarlagan; 49—Yanzigitovo; 50—Yanzigtovo II; 51—Koltuban; 52—Fayzullino; 53—Mambetovo; 54— Baltatau

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scrapers, micro scrapers, and side scrapers on plates. Most of the finds of the site are associated with the Neolithic layer. These are numerous flakes, nuclei, and chips from them and finished tools with two-sided processing: knives made of flint and jasper tiles and green siliceous tuffite. Axes and adzes for wood processing were also found there (Matyushin 1973). Mesolithic sites are also known on the Sabakty, Surtanda, and Chebarkul lakes, located south of the Mysovaya campsite (Matyushin 1976). The Kryktytau and Irendyk ridges are dissected by transverse valleys of streams and small tributaries of the Kizil and Urtazymka Rivers. In these streams, at the exit from the mountains, alluvial fans are formed with numerous outcrops to the surface of pebble and small-boulder material, represented mostly by the strong, most resistant to weathering rocks: jasper-like siliceous shale. One of such pebble outcrops was mapped by the author on the western side of the (dry) lake Sagylkul (author’s name) (Kazakov 2017; 2020). These outcrops of jasper pebbles belong to the ancient (the Middle-Late Neopleistocene) alluvial fans of the Karasaz River, which at a later time changed the direction of its channel from latitudinal (transverse to the Irendyk ridge) to meridional (2–3 km west of the Sagylkul Lake). Outcrops of pebble material are traced along the right side of the river valley Karasaz and upstream at 4.5 km NW of the lake Sagylkul. Here, within the Baishevsky archaeological district (AMD), there is the Sarytash site. It is worth researching interest in terms of the use of stone material by ancient people. At the Sarytash site in 1996 and then in 2003, nineteen stone products made of gray-green jasper were collected: a chopping tool, bumpers, prismatic single-site nuclei, and one radial cleavage nucleus, as well as numerous chips, flakes, and scrapers. This site (the location of “Sarytash-1b”) belongs to the type of Paleolithic workshop located next to the source of jasper pebbles. Its artifacts mostly date back to the Middle Paleolithic (Kotov and Savelyev 2001, p. 88). Also, within the Baishevsky AMD in the upper reaches of the river Bolshaya Urtazymka (Urgaza), in a narrow mountain valley, a stone-working site workshop Kyzyl-Yar 2 was found. It is confined to a rocky outcrop of green jasper, the surface of which is covered with negatives of large chips for several tens of meters and to a height of 4 m. The pit, laid near the rock, contains a large collection of chips and tools of the Mousterian era, including scrapers, large chopping tools, and jasper cores. Nearby, at the outlet of the channel alluvium, consisting of jasper pebbles and large pieces of green jasper, two more similar workshops were found—Kyzyl-Yar 4 and Yumash-Tau 8. Numerous spalls, large blocks of jasper with separate spalls, cores of radial spalling, two large prismatic cores, and chopping tools (Akbulatov et al. 2004, p. 297).

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4 Conclusions 1. Resource assessment of ferromanganese deposits in the Jasper Belt of the Southern Urals, along with the remaining reserves of oxidized ores, is associated with primary manganese-siliceous ores. 2. Gold ore deposits are localized in the jasper of the Yarlikapov horizon in the areas of brecciation and intensive silicification of siliceous shales. The relationship between the gold placers of the East-Irendyk zone with the horizons of mineralized jasper has been established. 3. The saturation and diversity of the flint material of the jasper belt of the Southern Urals, combined with favorable landscape and climatic conditions, contributed to the successful settlement of ancient people and the development of the stone industry. 4. The use of the unique natural resources of the Jasper Belt by a man from the Stone Age to the present is a reference point for further geoarchaeological studies of the region. Acknowledgments The work was performed within the framework of the State Contract (02522017-0012).

References Akbulatov, I.M., Akhtaryanova, D.I., Kotov, V.G., Mineeva, I.M., Savelyev, N.S.: Arkheologicheskiye otkrytiya 2003 (Archaeological discoveries 2003) Institut arkheologii (Institute of Archaeology), 527 p. Moscow, Nauka (2004) (in Russian) Bader, O.N., Matyushin, G.N.: Novyj pamyatnik srednego paleolita na Yuzhnom Urale. Sovetskaya arkheologiya (A new monument of the middle Paleolithic in the Southern Urals). Sovetskaya arheologiya (Soviet Archaeology) 4, 135–142 (1973) (in Russian) Betekhtin A.G.: Yuzhnoural’skiye margantsevyye mestorozhdeniya kak syr’yevaya baza Magnitogorskogo metallurgicheskogo kombinata imeni Stalina (South Ural manganese deposits as a raw material base of the Stalin Magnitogorsk Metallurgical Combine) Trudy Instituta geologicheskikh nauk Akademiya nauk SSSR. Seriya rudnykh mestorozhdeniy (Proceedings of the Institute of Geological Sciences Academy of Sciences of the USSR. A series of ore deposits), 30, 64 p (1940) (in Russian) Fersman, A.Y.: Ocherki po istorii kamnya (Essays on the history of the stone) vol. I, 371 p. Moscow, Academy of Sciences of the USSR Publ. (1954) (In Russian) Gusev, S.V., Zagorulko, A.V., Mineeva, I.M., Ozheredov, Y.I.: Arkheologicheskie muzei zapovedniki Rossiiskoi Federatsii: Problemy formirovaniya i funktsionirovaniya. (Archaeological Museum Reserves of Russian Federation: Problems of Formation and Functioning). Tom I: Evropeiskaya chast’ Rossii (Vol. I: European Part of Russia), 256 p. TML-Press Publ., Tomsk (2010) (in Russian) Humboldt, A.: O kolichestve zolota, dobyvayemogo v Rossiyskoy imperii (About the amount of gold mined in the Russian Empire) Gornyy zhurnal (Mining Journal) 1, 412 (1830) (in Russian) Kazakov, P.V.: Ostatochnye ozera N–Q paleogidroseti, ozernye kompleksy i soputstvuyushchie im poleznye iskopaemye (vostochnyi sklon Yuzhnogo Urala i Zaural’e) (Residual lakes of the N– Q paleohydronet, lacustrine complexes and associated minerals (eastern slope of the Southern

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Urals and the Trans-Urals)). Geologiya. Izvestiya Otdeleniya nauk o Zemle i prirodnykh resursov Akademii nauk Respubliki Bashkortostan (Geology. Proceedings of the Department of Earth and natural resources Sciences of the Academy of Sciences of the Republic of Bashkortostan). 23, 63–68 (2017) (in Russian) Kazakov, P.V.: New Objects of Geoarchaeology of the Baishevsky Archaeological District and the Adjacent Territory of the Bashkir Trans-Urals (The Southern Urals). In: Ankusheva N., Chechushkov I.V., Stepanov I., Ankushev M., Ankusheva P. (eds.) Geoarchaeology and Archaeological Mineralogy. GAM 2020. Springer Proceedings in Earth and Environmental Sciences, pp. 104–116. Springer, Cham (2022) Kotov, V.T., Savel’ev, N.S.: Novyj paleoliticheskij pamyatnik v Bashkirskom Zaural’e (New Paleolithic monument in the Bashkir Trans-Urals). Ufimskij arheologicheskij vestnik (Ufa Archaeological Bulletin) 3, 88–93 (2001). (in Russian) Matyushin, G.N.: Mezoliticheskij i neoliticheskij kompleksy poseleniya Mysovogo na Yuzhnom Urale (Mesolithic and Neolithic complexes of the settlement of Mysovoye in the southern Urals). Sovetskaya arheologiya (Soviet Archaeology) 4, 143–159 (1973). (in Russian) Matyushin, G.N.: Mezolit Yuzhnogo Urala (Mesolithic of the South Urals), 368 p. Moscow, Nauka (1976) (in Russian) Menshikov, V.G., Kazakov, P.V., Boikov, G.V., Greshilov, A.I.: Korennaya i rossypnaya zolotonosnost’ Respubliki Bashkortostan (Ore and loose gold of the Republic of Bashkortostan) Otechestvennaya geologiya. (Domestic Geology) 7, 20–26 (1997) (in Russian) Salikhov, D.N., Kovalev, S.G., Brusnitsyn, A.I., Belikova, G.I., Berdnikov, P.G., Semkova, T.A., Sergeyeva, Ye.V.: Poleznyye iskopayemyye Respubliki Bashkortostan (Mn) (Mineral resources of the Republic of Bashkortostan (manganese)), 243 p. Ekologiya Publ., Ufa (2002) (in Russian) Salikhov, D.N., Kovalev, S.G., Sharafutdinova, L.A.: Poleznyye iskopayemyye Respubliki Bashkortostan (dekorativno-podelochnyye kamni). (Mineral resources of the Republic of Bashkortostan (decorative and ornamental stones), 247 p. DizaynPoligrafServis Publ., Ufa (2012) (in Russian)

Stone Products of Prestigious Technologies on the Sites of the Stone and Bronze Age of the Urals Yu B. Serikov

Abstract Prestigious technologies are focused on the manufacture of products for public display. Their purpose is not to solve practical problems but to demonstrate wealth, prestige, status, and power. Prestigious products may include tools or jewelry made with extraordinary skills, having an unusual shape and large dimensions. They were often made from rare and spectacular types of mineral raw materials. The complexity in the manufacture of such items was important. From the Upper Paleolithic to the Early Iron Age, stone products of prestigious technologies were used in all archaeological periods. In the Urals, shaped hammers, maces, “ironings,” flint sculpture, jade, and rock crystal products are considered prestigious. Keywords The Urals · Prestigious technologies · Shaped hammer mace · “Ironings” flint sculpture · Jade · Rock crystal

1 Introduction The concept of prestigious technologies has begun developing in the last quarter of the XX century. The purpose of such technology is not aimed at practical tasks but at demonstrating wealth, prestige, status, and power. Among the stone products, prestigious items include items that differ in the thoroughness of manufacture, have an unusual shape, and have large dimensions. Rare and spectacular (sometimes imported) types of mineral raw materials were often used in their manufacture (Lbova and Tabarev 2009, p. 110–111). The labor intensity in producing such items was also one of the conditions for increasing their status level. The more time and labor was spent on manufacturing, the higher their social status became (Serikov 2018). Such products were intended to demonstrate the status and prestige of their owners and could be used during special rituals and ceremonies. On the territory of the Urals, products of prestigious technologies have been known since the Upper Paleolithic. But they were more widespread during the Neolithic and the Bronze Age. Y. B. Serikov (B) Russian State Professional Pedagogical University (Nizhny Tagil Branch), Nizhny Tagil, Russia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 N. N. Ankusheva et al. (eds.), Geoarchaeology and Archaeological Mineralogy—2021, Springer Proceedings in Earth and Environmental Sciences, https://doi.org/10.1007/978-3-031-16544-3_7

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This paper presents the first results of identifying and attributing products of prestigious technologies during the Stone and Bronze Ages in the Middle TransUrals.

2 Materials and Methods The technological method determines the sequence and content of actions to perform shaping and processing. The mineralogical method allows determining the type, properties, and characteristics of the minerals and rocks used to create objects. Prestigious artifacts considered in the article are made of slate, jasper, talc, jade, and rock crystal. With the help of use-wear analysis, the manufacturing technique and the tools’ functions have been attributed. The data obtained have been confirmed by an experimental study that showed labor costs and techniques for making objects. Their manufacturers used retouching, chipping, grinding, and drilling techniques. Experiments have shown that manufacturing large-diameter holes using a tubular bone or a copper tube is the most labor-intensive operation (Serikov and Grekhov 2021).

3 Results and Discussion In this paper, the author examines some ancient objects, which he refers to as the products of prestigious technologies. 1. The shaped hammer of greenish talc in the form of an elk head comes from the Neolithic settlement of Yevstyunikha I (the area of Nizhny Tagil, Sverdlovsk Region, Russia). The hammer is 8 cm long, 4.2 cm high, and up to 4.6 cm wide. The image is characterized by realism: it emphasizes a humped nose with nostrils and a thick saggy lip. A thin circular groove surrounds the eye. There is a small ledge on the back of the head, probably the remains of the lost ears. A 4.2 cm long hole in the shape of a truncated cone runs through the center of the product. The upper part has a diameter of 1.4 cm, and the lower part’s diameter is 1.8 cm (Fig. 1a). The hole is obtained by unilateral drilling with a tubular bone. Drilling was performed from the underside of the hammer. The entire surface of the hammer is well sanded and thoroughly polished. Shaped stone hammers are known in the Middle and Southern Urals in 9 items. They are made of talc, serpentinite, diabase, granite, and quartzite sandstone. Undoubtedly, the complexity of manufacturing such items was one of the conditions for increasing their status level. All this makes it possible to attribute shaped hammers to products of prestigious technologies, the main task of which was to demonstrate prestige, status, and power (Serikov 2018, p. 58).

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Fig. 1 Prestigious products of the Stone and Bronze ages: a shaped hammer in the form of an elk head (Evstyunikha I); b a billet of a jade mace (Ust’ye I); c a crystal mace (the Kizilskoye settlement); d a billet of a crystal mace (the Sunduk River)

2. The rarest find is the pommel of a mace in the form of a quartz ball. It was found in one of the mounds of the Kizilskoye settlement of the Bronze Age (the Chelyabinsk region). The mace lay at the base of the chest of the deceased. The ball has the shape of a uniaxial ellipsoid with a diameter of 5.7 cm. Its height is 3.5–3.8 cm. In the center of the ball, there is a conical hole with a diameter of 1.9 cm in the wide part and 1.1 cm in the narrow part (Fig. 1c). The ball is carefully treated with an abrasive. It is made of a big monocrystal of semitransparent quartz. With directional lighting, it accumulates light and sparkles. Yushkin (2005) believed that the spectacular bright radiance of the ball

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might indicate its ritual purpose. He emphasized that a large and transparent crystal was needed to make such a ball, which is quite rare. The processing of the artifact (grinding and drilling) required special skills and a lot of labor. 3. Another “mace” made of rock crystal with an unfinished drilled recess comes from the Sunduk River in the former Orsk district (Fig. 1d) f. The largest diameter of the mace is 5.5 cm, the smallest is 3 cm, and the height is 4.2 cm. The diameter of the unfinished drill is 2 cm. The drilling depth is 0.5 cm. Interestingly, this hole is not made with a hollow drill (bone or copper tube), as maces and shaped hammers were usually drilled. Instead, a massive stone drill was used. The product is processed by the picketing technique with subsequent surface polishing. According to the author, this is not a mace but a tool that served as an emphasis when producing fire by the archer method. Such a tool could be used in rituals for obtaining sacred fire (Panina 2004, p. 256). 4. A unique product was found in the Bronze Age fortified settlement of Ust’ye I (the Chelyabinsk region). This artifact is a billet of a mace made of dark green jade measuring 6.3 × 7.1 × 4.25 cm (Fig. 1b). The mace has two relief ledges (out of four) in one plane, roughly processed with an abrasive stone saw (Drevnee… 2013, p. 186–188). The origin of the jade has not been found. But considering that this is a single artifact, besides the fact that it is unfinished, it can be assumed that a rich-green rolled piece of jade was found in one of the local pebbles. The master, who did not know about the complexity of jade processing, left the product unfinished. Nevertheless, even an unfinished mace was a product of prestigious technologies. 5. The ancient calendar is an unusual object found in the vicinity of Nizhny Tagil Town (the Sverdlovsk region of Russia). It is made in the form of a large ovalshaped disk. The length of one axis is 14 cm, and the second one is 11.8 cm. The disc thickness is 1.5 cm (Fig. 2a and b). It is made of soft rock such as clay shale. All surfaces—front, back, and edge—are carefully sanded. There is a round hole in the center of the disc with a 3.5–3.7 cm diameter. It is formed by two-way picketing. Large notches are cut along the side faces of the disk on both sides with a metal tool (all other engravings are made with a stone tool). The number of notches is not accidental: three notches are applied on the front side in one horizontal belt with a hole on both sides, and 30 notches are located in the upper semicircle and 20—in the lower one. On the reverse side, 4 and 3 notches are applied on both sides of the hole, in the upper semicircle—28 and the lower—26 notches. There is an ornament in the form of a zigzag line on the edge of the disk. There are short notches on both sides opposite the hole, and on one side, there are also paired notches. The same zigzag line (but double) is applied on the reverse side of the disk. It runs along the entire disk perimeter along the face ornamented with notches. Below the zigzag is a more complex ornament in the central part of the plane. It consists of obtuse angles connected by beams. There is a gap in one place where the beams do not connect. There are paired notches at the top of each corner (except for one). There are 12 such corners, in total. Long paired notches are applied around the hole in the vertical and horizontal planes.

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Fig. 2 Prestigious products of the Eneolithic era: a, b disk-calendar (Nizhny Tagil); c, d “ironing” with a casting mold (Shaitan Lake I)

Two fantastic anthropomorphic creatures are depicted on the front side of the disc. One of them is standing, and the other is lying. A standing anthropomorphic shows a head, neck, arms, torso, legs, and tail. The head consists of a rhombus and two corners under it. The broad shoulders end in paired notches, the arms hang down from the shoulders, and they are three-toed. A long pole (?) stretched horizontally from the elbow of the left hand, on which three pairs of notches were applied at regular

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intervals, facing down. There are 8 notches on the torso, apparently depicting ribs. Both legs, as well as the hands, are three-toed. Moreover, one long finger opposes two shorter ones. The head of the reclining anthropomorphic is shown by two pairs of notches facing in different directions. Its shoulders and arms are the same as the first figure. The trunk has seven notches (ribs), and the tail is marked with a zigzag (Fig. 2a). The study of the disk surface revealed several areas with traces of strong burnishing. The side faces of the product with notches turned out to be highly polished. It seems that they were led by a finger when counting. The depiction of both figures is so unusual that they can be interpreted as costumed anthropomorphs (shamans, sorcerers) or as pangolins. There are no engraved images of anthropomorphic figures among the stone engravings on the territory of the Urals. However, there is a distant resemblance to the anthropomorphic figures carved on the back of a Large Shigir idol. Individual elements of the engraved images of the disk are well represented on the engravings of bone Mesolithic arrowheads. These are zigzag lines; zigzags, at the vertices of the corners of which there are paired notches; zigzags of segments intersecting with each other (Chernetsov 1971, Fig. 60; Serikov 2000, Fig. 125–129). The closest analogies to the engraved anthropomorphic figures can be found among the rock images of the Urals (Irbit Pisaniy Stone, Tagil Pisaniy Stone (Chernetsov 1971, Fig. 8, 51). But the published images have only a distant resemblance to the above analogies. It can be assumed that both figures depict shamans dressed in ritual costumes of a man-beast. The functional and sacred purpose of this subject requires special research. Considering the number of notches on the edges of the disk, it can be assumed that it was a kind of calendar that served to record and determine different astronomical phenomena (Gerasimenko 2004). Judging by the analogies and engraving technique, the disk can be dated to the Eneolithic—Early Bronze Age. 6. So colled “ironings”—are mysterious objects, the functional and sacred purpose of which is still debatable. Their distinguishing feature is a transverse groove and, as a rule, rich ornamentation. “Ironings” are widespread both in the territory and in time. They are known in the territory from Moldova to Mongolia and from North Africa to the taiga zone. Their greatest concentration is recorded in Ukraine, the Urals, and the Middle East. About 450 “ironings” have been identified in this territory by Usacheva (2013). They existed from the Mesolithic to the Middle Bronze Age Seven such objects were found in the Eneolithic cult center of Shaitan Lake I. One of them is a unique product (Fig. 2c and d). It is made in a pie form with its corners cut off. Its upper plane is convex, the end surfaces are smooth, and the corner of one of them is broken off. The lateral planes are inflated. The object’s length is 12.5 cm, the width is 7.7 cm, and the height is 3.5 cm. Unlike other “ironings,” it has two grooves of 1 and 1.2 cm in diameter. Concerning the object’s longitudinal axis, the grooves are not perpendicular but slightly angled. On the lower surface of the “ironing,” there is a shallow recess 7.5 cm long and up to 2.1 cm wide. It remains unclear how the object

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was made since traces of processing are not visible. According to the preliminary determination, the recess was used as a casting mold. As a result, the melting of its inner surface destroyed all traces of processing. The lower and side surfaces of the “ironing” are decorated with carved lines located at an angle to the longitudinal axis of the product. The end planes are not ornamented. The upper surface of the ironing is also covered with carved lines. Still, here they already represent a certain composition: they are arranged in groups located at different angles to each other (Fig. 2c). The “ironing” is made of light gray soft slate (Serikov 2013, p. 29). It should be noted that among the 450 identified “ironings,” molds on the lower surface are cut out only on the three “ironings.” One “ironing” with a mold for casting a flat adze was found at the site of Uly-Zhilanshik (Kazakhstan). In addition to the casting mold, a human face is additionally carved on the end protrusion of the “ironing.” The second “ironing” comes from the hoard on the site “Martishkina Balka” (the Rostov region of southwest Russia). Massive “ironing” with a length of 20.2 cm of the upper plane has two threaded grooves. And in the lower part, a casting mold for casting a flat adze is cut out (Serikov 2019, p. 14). The consistency of the form and design of the “ironings” indicates the similarity in their function and their use as religious objects. The decoration of the “ironings,” sculptural images, casting molds, and their placement in burial complexes, hoards, and sanctuaries, prove that these mysterious objects served to perform important sacred functions and belonged to persons of high social status. 7. The rosk crystal nucleus was found at the Mesolithic settlement of Sery Kamen— the old site of the Gorbunovsky peat bog (the vicinity of Nizhny Tagil, the Sverdlovsk region). It is the only crystal product among the nine thousand objects in the settlement collection. It lay down in the dwelling next to the hearth. The cone-shaped nucleus with a height of 2.9 cm is made of the purest rock crystal. The impact pad has the shape of an oval measuring 1.9 × 1.6 cm. Narrow knifeshaped plates were chipped from it along the entire perimeter. Seventeen negatives were recorded from the removal of plates with a width of 0.25–0.35 cm (Fig. 3a). The lower part of the nucleus was damaged by a chip that violated the correct shape of the product. Due to the numerous facets that create an original optical effect, the nucleus is perceived as a unique product of clearly sacred purpose (Serikov 2014, p. 154). It can be confidently attributed to the products of prestigious technology. The purity of the raw materials and the optical effect made this unique product quite a suitable subject for performing rituals. 8. The site of Murino I is located on the shore of the Murinsky Pond within the Nizhny Tagil area. The site has multiple phases; it contains materials from three archaeological ages. In the Eneolithic complex, two knives made of red-green jasper are distinguishable by their raw materials and processing techniques. The dimensions of the first knife are 6.5 × 3.3 × 0.45 cm. Moreover, the thickness of the knife decreases to 0.3 cm on its edges. There is a small break at the upper end. One side of the knife (front) is treated with a flat stream retouching. On the opposite side, a tiled crust has been preserved. All the side edges and end ends of the

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Fig. 3 Prestigious Mesolithic—Eneolithic products: a crystal nucleus (Sery Kamen); b jasper figure in the form of a goose paw (Sabakty 8); c, d knives made of red-green jasper (Murino I); e shaped “hammer” in the form of the head of a fantastic beast (Shigirsky peat bog)

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product were retouched. Only the lower (opposite to the breakout) end of the knife was treated with flat pressing retouching (Fig. 3d). In the middle of the front side is a strip of sealing wax with a width of 2.3 cm. There are green stripes along its edges. On the one side, their width is 0.5–0.9 cm. On the other side, the width is 0.3–0.4 cm. On the reverse side, a strip of sealing wax of up to 2.7 cm in width occupies the entire middle of the knife. The green stripes shifted to the edges of the knife; their width decreased to 0.4 cm on one edge and 0.5 cm on the other. The second knife, measuring 7.6 × 3.4 × 0.5 cm, is made with the same flat retouching and has the same color scheme. The only difference is that on one side, there is a spike in the form of a flat triangle with a height of 0.6 cm (Fig. 3c). Undoubtedly, both knives are made of the same piece of red-green jasper. 9. In the Eneolithic complex of the site Sabakty 8 on Sabakty Lake (the Bashkir Trans-Urals), a large stone object made in the form of a goose (?) paw was found. It is made on a flake of gray-green jasper measuring 10. 8 × 7. 9 × 2. 1 cm. The shape of the figure resembles the paw of a waterfowl and could be a bird symbol (Fig. 3a) (Kotov and Savelyev 2007). The large size and unusual shape of the sculpture allow us to see it as a prestigious product.

4 Conclusions All the analyzed items fully comply with the above criteria for determining the prestige objects. They are characterized by their original shape, unusual raw materials, and labor intensity in manufacturing. There are many more products of prestigious technologies in the archaeological complexes of the Urals than are presented by the author in this article. They were made not only of stone but also of other materials. It is enough to recall the inserted knife from the mammoth rib and the horn sculpture of a fantastic animal from the Shigir collection (Fig. 3e), shaped hammers, large ornamented discs, many “ironings,” some flint sculptures, arrowheads treated with fine sawn retouching from the burial at the site Koksharovo I, copper daggers with figured handles and a sword from Shaitan Lake II, stone poleax-shaped axes-hammers of the Bronze Age from the Southern Urals and some other products from different eras.

References Chernetsov, V.N.: Naskalnye izobrazheniia Urala (Rock paintings of the Urals). p. 120. Nauka, Moskva (1971) (in Russian) Drevnee Ust’e: ukreplennoe poselenie bronzovogo veka v Iuzhnom Zaural’e (Ancient Mouth: a fortified settlement of the Bronze Age in the Southern Transurals). p. 482. Abris, Cheliabinsk (2013) (in Russian) Gerasimenko, A.A.: Drevnii kalendar’ i kalendarnaia mifologiia naseleniia Srednego Zaural’ia (opyt interpretatsii odnoi nakhodki) (Ancient calendar and calendar mythology of the population of the

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Middle Transurals (experience of interpretation of one find)). Chetvertye Bersovskie chteniia (Fourth Bersov readings), 83–90 (2004) (in Russian) Kotov, V.G., Savelyev, N.S.: Eneoliticheskaia stoianka Sabakty-8 v Bashkirskom Zaural’e (The Eneolithic site Sabakty-8 in the Bashkir Transurals). Ufimskii arkheologicheskii vestnik (Ufa Archaeol. Vestn.) 6–7, 12–18 (2007) Lbova, L.V., Tabarev, A.V.: Kultura, iskusstvo, ritual. Proiskhozhdenie i rannie etapy: Uchebnoe posobie (Culture, art, ritual. Origin and early stages: A textbook). p. 142. Novosibirskii gosudarstvennyi universitet, Novosibirsk (2009) (in Russian) Panina, S.N.: Kultovye predmety v sobranii arkheologicheskikh kollektsii Sverdlovskogo oblastnogo kraevedcheskogo muzeia (Cult objects in the archaeological collections of the Sverdlovsk regional Museum of Local lore). Kultovye pamiatniki gorno-lesnogo Urala (Cult Sites Mt.-For. Urals), 255–256 (2004) (in Russian) Serikov, Yu.B.: Paleolit i mezolit Srednego Zauralia (Paleolithic and Mesolithic of the Middle Transurals). p. 430. Polygraphist, Nizhny Tagil (2000) (in Russian) Serikov, Yu.B.: Shaitanskoe ozero—sviashchennoe ozero drevnosti (Shaitanskoje Lake is a sacred lake of the Ancient time). p. 408. Nizhny Tagil State Social and Pedagogical Academy, Nizhny Tagil (2013) (in Russian) Serikov, Yu.B.: Ocherki po pervobytnomu iskusstvu Urala (Essays on the primitive art of the Urals). p. 268. Nizhny Tagil State Social and Pedagogical Academy, Nizhny Tagil (2014) (in Russian) Serikov, Yu.B.: K voprosu o tekhnike izgotovleniia otverstii bol’shogo diametra v kamennykh izdeliiakh neolita—bronzy Urala (On the question of the technique of making large-diameter holes in Neolithic—Bronze stone products of the Urals). Povolzhskaia arkheologiia (Povolzhskaya Archeol.) 1, 56–73 (2018) (in Russian) Serikov, Yu.B.: Predmety neutilitarnogo naznacheniia v kladakh kamennykh izdelii Urala i Sibiri (Objects of non-utilitarian purpose in the hoards of stone products of the Urals and Siberia). Narody i religii Evrazii (Peoples Relig. Eurasia) 1, 7–17 (2019) (in Russian) Serikov, Yu.B., Grekhov, S.V.: Eksperimental’noe modelirovanie otverstii bol’shogo diametra po materialam kamennykh toporov bronzovogo veka (Experimental modeling of large diameter holes based on materials of stone axes of the Bronze Age). Povolzhskaia arkheologiia (Povolzhskaya Archeol.) 3, 155–165 (2021) (in Russian) Usacheva, I.V.: “Utiuzhki’ Evrazii (“Ironins” of Eurasia). p. 352. Nauka, Novosibirsk (2013) (in Russian) Yushkin, N.P.: Kvartsevye shary v materialnoi kulture cheloveka (Quartz balls in the material culture of man). Arkhaeomineralogiia i ranniaia istoriia mineralogii (Archaeomineralogy Early History Mineral.), 74–77 (2005) (in Russian)

The Microstructure and Mineral Composition of Flint Artifacts at the Epipaleolithic of the Northern Caucasus: Preliminary ESM Results Vladimir A. Tselmovich and Ekaterina V. Doronicheva

Abstract Scanning electron microscopy (SEM) with energy dispersive spectrometers (EDS) was performed on samples from chert outcrops and 31 chert artifacts from several Epipaleolithic sites, including the Sosruko and Psytuaje rockshelters in the North-Central Caucasus, and the Gubs VII rockshelter and Kasojskaya Cave in the North-Western Caucasus, dated at the end of the Last Glacial Maximum to the early Holocene. As a result, we defined several chert sources that Epipaleolithic huntergatherers exploited in the region. The SEM results mainly confirm the previous results obtained using petrography and geochemistry but also provide new data on raw material transport in the Northern region during the Epipaleolithic. The most important result is that some chert artifacts from the Epipaleolithic layer 7 at the Sosuko rockshelter are made from Cretaceous flint transported from the Besleneevskaya outcrops, located in the North-Western Caucasus, about 250 km linearly from the site. This supports the archaeological data indicating the lithic and bone artifacts from layer 7 are analogous to the Epipaleolithic of the North-Western Caucasus. Keywords Raw material procurement · Geochemistry · Scanning electron microscopy · Chert artifacts · North Caucasus · Epipaleolithic

1 Introduction The study of raw material sources and transportation routes provides new data on lithic raw material strategies and technological achievements of the Paleolithic populations in different regions and various periods (e.g., Féblot-Augustins 1993; Spinapolice 2012; Hughes et al., 2016; Moreau et al. 2016, 2019; Sánchez de la Torre et al. 2017a, 2017b, 2020; Brandl et al., 2018;). Our previous results indicated that V. A. Tselmovich (B) The Branch of Schmidt Institute of Physics of the Earth of the Russian Academy of Sciences, Borok Geophysical Observatory, Borok, Russia e-mail: [email protected] E. V. Doronicheva Laboratory of Prehistory, St.-Petersburg, Russia © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 N. N. Ankusheva et al. (eds.), Geoarchaeology and Archaeological Mineralogy—2021, Springer Proceedings in Earth and Environmental Sciences, https://doi.org/10.1007/978-3-031-16544-3_8

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the Epipaleolithic hunter-gatherer groups in the Northern Caucasus applied complex strategies to procure, transport, and use different lithic raw materials, including flint and obsidian (Doronicheva et al. 2012, 2013, 2019). Scanning electron microscopy (SEM) is currently widely applied to analyze various samples in archaeology (Ponting 2004). In this study, we apply SEM to analyze flint samples from some major chert outcrops and several Epipaleolithic sites in the Northern Caucasus to study raw material procurement and transportation. The SEM data on the chemical composition of microinclusions in flint samples provide new evidence on the lithic raw material strategies of Epipaleolithic hunter-gatherers and indicates contacts with remote regions in that period.

2 Materials and Methods Siliceous rocks, including chert, have a biogenical origin through dissolution and redeposition of carbon dioxide, sulfate ions, and other components included in the skeletons of radiolarians, diatoms, and sponge spicules (Kuznetsov and Proshlakyov 1991). Many studies show that the composition of flint can vary within the same geological deposit, while flint samples from different deposits may have a similar composition. Essential differences that appear during the formation of flintbearing deposits are related to the composition and number of microinclusions and microstructure. To obtain more reliable results for our study, we collected several samples from each flint outcrop that we sampled in the Northern Caucasus. Since 2007, one of us (ED) has created the reference collection of lithic raw material source standards (lithotheque) of mainly siliceous rocks from outcrops in the Northern Caucasus, which now consists of more than 1,000 samples from 65 outcrops and is stored in the Laboratory of Prehistory in St.-Petersburg, Russia. Accepting ten outcrops located in the North-Central (NC) Caucasus, 55 outcrops are located in the North-Western (NW) Caucasus. Chert, including flint, outcrops from the NorthEastern Caucasus are not studied at all at present. For this research, we use source standards from some of the chert outcrops sampled earlier in the region. To define the morphology and chemical composition of chert samples by SEM, we used an Olympus BX-51 metallographic microscope (in bright field mode) equipped with a photo camera and a Tescan Vega II scanning electron microscope equipped with devices for energy dispersive X-ray microanalysis (EDS). The flint samples were sawn off with a diamond saw, poured with Wood’s alloy (Sn-Pb-Bi-Cd) in a brass washer (26 mm in diameter), and then ground and polished. Using a conductive Wood’s alloy reduces sample charge, improving image quality and chemical analysis. All samples were analyzed firstly using a portable USB microscope at low magnification and then with an Olympus BX51 microscope. This preliminary analysis identified the main differences in structure, texture, and micro- and macroinclusions in the samples. In the second stage, the samples were deposited with carbon in an Emitech K550X vacuum device for a more detailed analysis using SEM. These methods produced detailed information about the mineral composition

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of impurities and inclusions and defined fine structural and textural features inside the flint samples, allowing us to better distinguish textural features characteristic of each chert-bearing geological deposit. The EDS spectra were processed using the INCA software package (Oxford Instrument Analytical Ltd., UK). SEM images of characteristic features in the analyzed samples were obtained. For this study, we analyzed 40 samples from primary chert sources known in the NC and NW Caucasus that include in the NC Caucasus, the 11 samples from the Shatauchukua-1 (1), Hana-Haku-1 (1), Baksan-1 (1), Chegem-1 (2), Kamenka-1 (4), and Cherek-1 (2) outcrops in the Elbrus region (Fig. 1). In the NW Caucasus, the 29 samples from Medvezhegorsk (2), Gamovskaya Balka-1 and -2 (2), Azish-Tau-1 and −2 (2), Gubs-1 and −2 (2), Ahmetovskaya (1), Besleneevskaya-1 and −2 (2), Shahan-1 and −3–5 (4), Shedok-1 (1), Fars-1 (1), Semiyablonya-2 (1), Meshoko-1 and −2 (2), Rufabgo-1 (1), Unakoz 1–5 (5), Baranakha-1 (1), Berezovaya Balka-1 (1), and Psebay-1 (1) outcrops (Fig. 2). Also, we analyzed 31 chert artifacts from the Epipaleolithic sites (Fig. 3) in the Northern Caucasus, including the Sosruko rockshelter, layers 8 (13) and 7 (5); the Psytuaje rockshelter, layer 2 (7); the Gubs VII rockshelter, horizon 4 (3); and Kasojskaya Cave, horizon 4 (3). The study of polished sections on archaeological chert samples was conducted with optical microscopes and scanning electron microscopes with EDS. The microscope analyses showed a great variety of the analyzed samples in color; red and dark red colors predominate. SEM studies showed that the coloration is caused by various oxides and hydroxides of iron that varied both in the oxidation degree and the size of micro- and nanoparticles. The bulk X-ray phase analysis (XRD) results showed that the sample consists mainly of quartz. In the samples analyzed, we identified micro-structures and micro-inclusions typical for specific chert sources (Fig. 4). Using SEM, it was also possible to better define the mineral composition and specific morphological features, such as porosity and the presence of carbonates, fossil fragments (apatite), silicate coccoid, pyrite, and magnetite framboids, of the samples.

3 Results and Discussion The main characteristics of chert-bearing deposits are shown in Table 1. For chert outcrops in the NC Caucasus, the results indicate that the silicate coccoid is typical only for the Kamenka-1 source, pyrite framboids are found in the Chegem-1 and Cherek-1 sources, and magnetite in the Baksan-1 source. The largest number of dispersed carbonates is identified in Cherek-1 and Chegem1, in a small amount in Kamenka-1 and Baksan-1, and is entirely absent in the Hana-Haku-1 and Shtauchukua-1 sources. Fossil fragments (apatite) are found in all sources studied in this region. Also, copper minerals are found only in samples from the Hana-Haku-1 source. The samples being studied from chert outcrops of the NW Caucasus can be divided into three groups:

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Fig. 1 SEM results for the most representative samples from chert sources in the North-Central Caucasus: a Shtauchukua-1, b Hana-Haku-1, c Baksan-1, d Chegem-1, e Kamenka-1

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Fig. 2 SEM results for the most representative samples from chert sources in the North-Western Caucasus: a Azish Tau-2, b Azish-Tau-1, c Gubs-2, d Semiyablonya-2, e Besleneevskaya, f Besleneevskaya-1, g Shahan-1, h Shahan-3, i Shahan-5

1—the Psebay-1 outcrop, with specific features of the presence of pyrite framboids (bacterial structures) and numerous carbonates (calcite). 2—Medvezhegorsk, Gamovskaya Balka-1 and -2, Azish-Tau-1 and -2), Besleneevskaya-1 and -2, Shahan-1, -3–5, Fars-1, Meshoko-1, Rufabgo-1, Unakoz 1–5, and Berezovaya Balka-1. For all chert sources of this group, carbonates (calcite), structures of bacterial mats, barite, and coccoid are characteristic. 3—the Ahmetovskaya outcrops are distinguished by the absence of carbonates.

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.Fig. 3 Archaeological chert samples from Epipaleolithic sites: a Sample 4, the Sosruko rockshelter, layer 8. (1) images obtained by Olympus BX51; (2–3) SEM images obtained by Tescan. Characteristic minerals: apatite, quartz, faunal remnants with small inclusions of calcium; porphyry structure; mottled texture. Assigned to the Shtauchukua-1 source. b Sample 23, the Psytuaje rockshelter, Layer 2. (1) images obtained by Olympus BX51; (2–3) SEM images obtained by Tescan. Characteristic minerals: quartz, ilmenite-rutile, hematite, and faunal remains; afanite structure; spotty texture. Assigned to the Baksan-1 source. c Sample 18, the Sosruko rockshelter, layer 7. (1) images obtained by Olympus BX51; (2–3) SEM images obtained by Tescan. Characteristic minerals: quartz, calcite on the borders, and faunal remnants in pores; afanite structure; spotty texture. Assigned to the Besleneevskaya sources. d Sample 27, the Gubs rockshelter VII, horizon 4. (1–2) images obtained by Olympus BX51; (3–4) SEM images obtained by Tescan. Characteristic minerals: quartz, hematite, faunal remains; porphyry structure; spotty texture. Assigned to the Shahan-4 source. e XRD graph showing quartz lines

To define the provenience of artifacts, the data on 31 archaeological chert samples from Epipaleolithic sites in the region were compared with the data on chert outcrops. Based on the results of microscope analysis, all archaeological chert samples can be divided into two groups, according to their structural and textural features identified (1) samples with large magnetite phenocrysts (porphyritic structure); (2) samples with an opaque, banded, and fluid texture. In some samples, both structuraltextural types are found. All archaeological chert samples being studied have a quartz matrix (Fig. 3e) and an insignificant number of micro-inclusions. The archaeological chert samples showing similar mineral composition and morphological features can be divided into five groups: 1. Relatively homogeneous samples, with few inclusions, and the microstructure formed by fossil fauna remains. 2. Samples that contain isomorphic grains of hematite. 3. Samples with framboidal pyrite or magnetite formed because of pyrite oxidation. 4. Samples that contain calcite. 5. Samples that contain spherical particles of hematite, FeCrNi alloy, and native copper in large pores. Microinclusions of titanium oxide and barite are also classified as diagnostic features in some samples. They also contain relatively large inclusions of faunal remains (apatite) and spherical particles.

4 Conclusions The new results obtained using SEM with EDS, in general, confirm previous data obtained using petrography and geochemistry on chert procurement in the Epipaleolithic of the Northern Caucasus (Golovanova et al. 2020, Doronicheva et al. 2020), but also provide new data. The results show that the 12 archaeological samples from the Sosruko rockshelter, layer 8 (13–16 kya), are derived from the Cretaceous

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Fig. 4 SEM images of specific microstructures in the analyzed archaeological chert samples: a pore with hematite ball, faunal remains (sample 3, Sosruko rockshelter, layer 7), b, c hematite in pores (sample 1, Sosruko rockshelter, layer 8 and Gubs 7 rockshelter, horizon 4), d–f faunal remains with different porosity (samples 7, 8, 10, Sosruko rockshelter, layer 8 respectively), g calcite inclusions (sample 11, Sosruko rockshelter, layer 8), h, i hematite inclusions (grey) (samples 13, 14, Sosruko rockshelter, layers 8 and 7 respectively), j—hematite inclusions on borders of pores and calcite inside pores (sample 26, Gubs VII rockshelter, horizon 4), k, l—particles of pyrite (light) with fayalite rim (sample 28, Gubs VII rockshelter, horizon 4, sample 30, Kasojskaya Cave, horizon 4 respectively)

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Table 1 Characteristics of nine chert sources in the Northern Caucasus Source

Characteristics

Shtauchukua-1

Foraminifera replaced with amorphous silica, large pores, and microspheres

Hana-Haku-1

Copper composition and mineralized shells of cyanobacteria

Baksan-1

Magnetite framboids, magnetite micrograins, calcite and barite in pores in the calcite matrix

+

Chegem-1

Many calcite, micrograins of bacterial pyrite and pyrite framboids

+

+

Kamenka-1

Amorphous porous silica, fine calcite, and pore-filled apatite

+

+

Cherek-1

Coarse calcite crystals, many carbonates, pyrite, framboids, hematite, and apatite

+

+

Besleneevskaya Barite oxide (BaSO4), traces of fauna (10–100 microns), hematite in the form of films and microcrystals, pyrite residues, brass (CuZn), remains of fauna, and traces of calcium

+

+

Azish-Tau-1

+

+

Frambo-hedral hematite, fauna remains, and calcite

Calcite Hematite Apatite Pyrite Fayalite Barite

+

+

+

+

+

+

+

+

+

(continued)

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Table 1 (continued) Source

Characteristics

Shahan-4

Apatite, pyrite with evidence of oxidation (holy rim on pyrite), rutile, and ilmenite

Calcite Hematite Apatite Pyrite Fayalite Barite +

+

+

Shatauchukua-1 outcrop, located 15–20 km linearly from the site, and one sample originates from the Cretaceous Kamenka-1 outcrop, located 25–30 km linearly from the site. A sample from the Sosruko rockshelter, layer 7 (~13 kya), was attributed to the Cretaceous Shatauchukua-1 outcrop (15–20 km linearly from the site) and one to the Besleneevskaya-1 outcrop of the Cretaceous period, located in the NW Caucasus (about 250 km linearly from the site). Archaeological research indicates that lithic and organic artifacts from layer 7 have analogies among Epipaleolithic assemblages in the NW Caucasus, including in the Epipaleolithic layer 1–3 at Mezmaiskaya Cave (Golovanova and Doronichev 2020). The analyzed archaeological chert samples from the Psytuaje rockshelter, layer 2 (11–13 kya), were probably procured locally. They were assigned to the Shtauchukua1 Cretaceous source (1), located about 7 km linearly from the site, as well as the Baksan-1 (2) and Kamenka-1 (2) sources, located about 10 km linearly from the rockshelter. In horizon 4 at the Gubs VII rockshelter, a single sample analyzed was assigned to the Shahan-4 outcrop, located ~ 20 km linearly from the site. The results show that the SEM with EDS can be successfully used to identify and refine some diagnostic features of samples from archaeological sites and natural sources. Acknowledgements The research was funded by Grant No. 17-78-20082 “Human-nature interaction in ancient in the Central Caucasus: dynamics of environmental change and technological innovations, and adaptations of subsistence strategies” (2020–2022) from the Russian Science Foundation. We thank Dr. Liubov Golovanova and Dr. Vladimir Doronichev for the possibility of working with materials from their excavations at the Sosruko rockshelter and Mezmaiskaya Cave. We also thank the anonymous reviewer, whose comments helped to improve the manuscript.

References Brand, M., Martinez, M.M., Hauzenberger, C., Nymoen, P.F., Mehler, N.: A multi-technique analytical approach to sourcing Scandinavian flint: provenance of ballast flint from the shipwreck “Leirvigen 1”, Norway. Published: August 8 (2018) Doronicheva, E., Kulkova, M., Grégoire, S.: La grotteMézmayskaya (Caucase de Nord): example de l’utilisation des matières premières lithiques au PaléolithiqueMoyenetSupérieur. L’anthropologie 116, 378–404 (2012)

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Doronicheva, E.V, Kulkova, M.A., Shackley, M.S: Exploitation of lithic raw material in the northwestern caucasus upper paleolithic. Archaeol. Ethnol. Anthropol. Eurasia 41(2), 40–53 (2013) Doronicheva, E.V., Golovanova, L.V., Doronichev, V.B., Shackley, S.M., Nedomolkin, A.G.: New data about the exploitation of the Zayukovo (Baksan) obsidian source in Northern Caucasus during the Paleolithic. J. Archaeol. Sci. Rep. 23, 157–165 (2019) Doronicheva, E., Golovanova, L., Doronichev, V., Nedomolkin, A., Shirobokov, I., Shackley, M., Petrov, A., Maksimov, F.: Psytuaje rockshelter—A new site documenting the final of the epipalaeolithic in the north-central caucasus Russia. J. Archaeol. Sci.: Rep. 29, 102186 (2020) Féblot-Augustins, J.: Mobility strategies in the Late Middle Paleolithic of central Europe and western Europe: elements of stability and variability. J. Anthropol. Archaeol. 12, 211–265 (1993) Golovanova, L.V., Doronichev, V.B.: Environment, culture and subsistence of humans in the caucasus between 40,000 and 10,000 years ago, 587 p. Cambridge Scholars Publishing, Newcastle upon Tyne (2020) Golovanova, L.V., Doronichev, V.B., Doronicheva, E.V., Tregub, T.F., Volkov, M.A., Spasovskiy, Yu.N., PetrovA.Yu., Maksimov F.E., Nedomolkin A.G.: Dinamique du climat et du peuplement du Caucase Nord-Central au tournant du Pléistocène et de l’Holocène (Dynamics of environment and human occupation of the north-central Caucasus at the edge of the Pleistocene and Holocene). L’Anthropologie 124,102759 (2020) Hughes, R.E., Werra, D.H., Suida, R.: On the chemical composition of flint from Central Poland. Archaeologia Polona 54, 99–114 (2016). PL ISSN 0066–5924 Kuznetsov, V.G., Proshlakyov, B.K.: Lothologiya (Lithology), pp. 143–146. Moscow, Nedra (1991) (in Russian) Moreau, L., Brandl, M., Filzmoser, P., Hauzenberger, C., Goemaere, É., Jadin, I., Collet, H., Hauzeur, A., Schmitz, R.W.: Geochemical sourcing of flint artifacts from Western Belgium and the German Rhineland: testing hypotheses on gravettian period mobility and raw material economy. Geoarchaeol. Int. J. 31, 229–243 (2016) Moreau, L., Ciornei, A., Gjesfjeld, E., Filzmoser, P., Gibson, S.A., Day, J., Nigst, P.A., Noiret, P., Macleod, R.A., Ni¸ta˘ , L., Anghelinu, N.: First geochemical «fingerprinting» of Balkan and Prut flint from Paleolithic Romania: potentials, limitations and future directions. Archaeometry 60(3), 521–538 (2019) Ponting, M.: The scanning electron microscope and the archaeologist. Phys. Educ. 39(2), 166–167 (2004) Sánchez de la Torre, M., Le Bourdonnec, F.-X., Dubernet, S., Gratuze, B., Mangado, X., Fullola, J.M.: The geochemical characterization of two long distance chert tracers by ED-XRF and LAICP-MS. Implications for Magdalenian human mobility in the Pyrenees (SW Europe). STAR: Sci. Technol. Archaeol. Res. 3(2), 15–27 (2017a) Sánchez de la Torre, M., Le Bourdonnec, F.-X., Gratuze, B., Domingo, R., García-Simón, L.M., Montes, L., Mazo, C., Utrilla, P.: Applying ED-XRF and LA-ICP-MS to geochemically characterize chert. The case of the Central-Eastern Pre-Pyrenean lacustrine cherts and their presence in the Magdalenian of NE Iberia. J. Archaeol. Sci.: Rep. 13, 88–98 (2017b) Sánchez de la Torre, M., Utrilla, P., Domingo, R.,Jiménez, L., Le Bourdonnec, F.-X., Gratuze, B.: Lithic raw material procurement at the Chaves cave (Huesca, Spain): a geochemical approach to defining Paleolithic human mobility. Geoarchaeology, 1–15 (2020) Spinapolice, E.E.: Raw material economy in Salento (Apulia, Italy): new perspectives on Neanderthal mobility patterns. J. Archaeol. Sci. 39, 680–689 (2012)

Ludogorian Flint as an Indicator of Manufacturing Relations Between the Sites of Kodjadermen-Gumelni¸ta-Karanovo VI (Chalcolithic, Bulgaria) Natalia N. Skakun, Chavdar Nachev, Boryana Mateva, and Vera V. Terekhina Abstract This work is devoted to studying flint-working production during the Chalcolithic in Bulgaria, where the dominant raw material is the high-quality largebouldered Ludogorian flint, common to the north-eastern regions of the country. The article presents its geo-mineralogical characteristics and considers the areas and nature of the widely exploited deposits, starting with the Chalcolithic. The study of the archaeological context at the mining sites and a comprehensive technical and morphological analysis of the flint inventory from various sites of that age indicated the presence of large workshops for the primary processing of nodules and their preparation for knapping in the vicinity of the flint deposits. The manufacture of tools from fragments of regular blades occurred at nearby settlements in specialized workshops, which were exposed during archaeological excavations at a number of sites. High-quality products from these workshops were widely used and were at the core of tool assemblages not only at most of the sites in Bulgaria and neighboring areas in Romania but also penetrated far to the north into the south-eastern regions of modern Ukraine. The research characterizes the Chalcolithic flint production in Bulgaria as highly specialized, focusing on the large-scale distribution of its products, which were in demand in the Balkan-Danube region due to their high quality. Keywords Chalcolithic · Kodjadermen-Gumelni¸ta-Karanovo VI · Ludogorian flint · Deposits · Extraction methods · Flint processing · Manufacturing relations

N. N. Skakun (B) · V. V. Terekhina Institute for the History of Material Culture, St.-Petersburg, Russia e-mail: [email protected] C. Nachev Independent Researcher, Sofia, Bulgaria B. Mateva National Polytechnic Museum, Sofia, Bulgaria © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 N. N. Ankusheva et al. (eds.), Geoarchaeology and Archaeological Mineralogy—2021, Springer Proceedings in Earth and Environmental Sciences, https://doi.org/10.1007/978-3-031-16544-3_9

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1 Introduction The Chalcolithic of the north-eastern part of the Balkan Peninsula is a complex phenomenon. It represents one of the first stages of a multicultural period, going back to the depths of the Late Neolithic cultures such as Hotnitsa II, Boyan II, and Usoe II, as well as the Golovitsa phase of the Hamangia culture. The general development trends since the Late Neolithic gradually led to the unification of these cultures, visible mainly during the Chalcolithic. During the early stages of the latter, the smooth progression does not allow for establishing an exact boundary between the two mentioned ages. The classical phases of the cultures corresponding chronologically to the Early Chalcolithic—Polyanitsa II–III and Hamangia III—are well represented in many tells in north-eastern Bulgaria. The Boyan III Vidra culture of south-eastern Romania is present very limitedly on the Bulgarian territory and was gradually absorbed by the Polyanitsa culture at the end of the Early Chalcolithic. All these early Chalcolithic cultures merged into a distinct cultural phenomenon at the beginning of the Late Chalcolithic—the Kodjadermen-Gumelni¸ta-Karanovo VI complex, which covered the entire north-east of Bulgaria. This phenomenon is culturally similar to the Varna culture on the Black Sea coast of Bulgaria (Todorova 1986). From the dawn of Bulgarian archeology, researchers drew attention to the great amount of high-quality flint in the north-eastern region of Bulgaria (Shkorpil and Shkorpil 1892; Popov 1928). Experts considered it the best raw material for the production of tools. They assumed that in ancient times the region of the Lom river basin was one of the main places for extracting flint raw materials in the Balkans (Kanchev et al. 1981; Nachev and Kunchev 1984; Skakun 1984, 1993; Nachev and Nachev 1989). The results of archaeological research indicate that large-scale mining of large-pebble northern Bulgarian flint (Ludogrian) began in the Chalcolithic (Com¸sa 1976; Kanchev et al. 1981; Skakun 1984, 1993, 1999, 2006; Todorova 1986). This study focuses on the organizational features of flint-working on the territory of North-Eastern Bulgaria during the Chalcolithic, characterizes the methods of Ludogorian flint extraction, and considers the types of workshops for flint processing and the production relations.

2 Materials and Methods The authors conducted comprehensive studies on several thousand flint artifacts from 22 sites of different periods of the Chalcolithic in Bulgaria (15 settlements), Romania (1 settlement), and six settlements of the Bolgrad-Aldeni II culture in Ukraine and Moldova. The information available in literary and archival sources (16 settlements) was also considered. The deposits of Ludogorian flint in the northeast of Bulgaria were examined, the available data on the properties of this raw material was

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used, and the results of archaeological, geological exploration, and the contexts of archaeological excavations were analyzed. Based on the archaeological data and the existing information on the flint raw materials, a unified technical and morphological classification of the Bulgarian Chalcolithic flint tool assemblages was created, which made possible the comparative analysis of products from different archaeological sites and the identification of their functional status as settlements that were producers of flint products and settlements that were consumers.

3 Results and Discussion Large-pebble North Bulgarian flint occurs in the Cretaceous deposits of the Aptian period of the Lower Cretaceous in the Ludogorie region in Northeastern Bulgaria. Primary deposits are found in the Cretaceous deposits along the banks of low-water river valleys, and colluvial deposits are especially typical for the Ludogorie Plateau region (the Razgrad and Samuil Hills, the Syrta and Stan Hill). Com¸sa (1976) labeled this type of flint as “Dobrudjian” based on the rich archaeological material from Romania. However, its distribution area is not restricted to the geographical region of Dobrudja, particularly the Dobrudja plateau. Subsequently, Kanchev (1985) proposed the term “Ludogorian flint.“ Still, although its deposits do coincide with the geographical boundaries of the Ludogorie region, in the literature, it continues some times to be called “Dobrudjian.“ In the Ludogorie region of Bulgaria, geologists have documented seven large deposits of this flint type (Nachev 2009, Fig. 1): 1. Near the city of Razgrad on the Razgrad Upland. 2. To the north-west of the city of Razgrad, in the valley of the Belyi Lom River, near the villages of Osenets, Dryanovets, Krivnya, Pizanets, and Nisovo. 3. To the north of the city of Razgrad, in the now dry valley of the Topchii River, in the Ruse and Razgrad regions, near the villages of Topchii, Kamenovo, Ravno, Belovets, and Tetovo. 4. In the Ruse region, in the valley of the Rusensky Lom and Cherny Lom (“Chukata”) rivers, near the villages of Nedoklan, and Mortagonovo, the Razgrad district. 5. To the south and south-west of the town of Isperikh, the Razgrad region, the Isperikh district, near the villages of Malak Porovets, Golyam Porovets, Vladimirovtsi, and Nozharovo. 6. To the north of the city of Novi Pazar, Shumen region, there is the most famous deposit at Krivareka, with outcrops near the villages of Lisivrah, Dolina, Ruzhitsa, Kharsovo, Stanovets, and Chernoglavtsi, the Shumen region. 7. The most eastern deposits are noted 40–45 km west of the city of Dobrich, in the Dobrich region, near the villages of Karapelit, Cherna, and Zhitnitsa. Ludogorian flint nodules have a well-defined thick pebble crust (6–12 mm); the color is yellowish-brown (honey, waxy), yellow, beige, and very rarely gray (Fig. 2)

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Fig. 1 Map of the location of the places of mining, processing, and use of Ludogorian flint in the Chalcolithic sites of Bulgaria and Romania. 1—Tetovo; 2—Dryanovets; 3—Kamenovo-Ravno; 4—Topchii; 5—Nedoklan; 6—Chukata; 7—Chakmaka; 8—Krivareka; 9—Kamenovo; 10—Chakmaka I; 11—Ruse; 12—GolyamoDelchevo; 13—Polyanitsa; 14—Provadiya-Solnitsata; 15— Ovcharovo; 16—Kosharna; 17—Demir baba teke; 18—Sredoseltsi; 19—Durankulak; 20—Kojadermen; 21—Sushina; 22—Vinitsa; 23—Hotnitsa; 24—Yunatsite; 25—Kazanlak; 26—Dyadovo; 27—Dolnoslav; 28—Pietrele; 29—Mariutsa; 30—Kosharna necropolis; 31—Varna necropolis; 32—Durankulak necropolis

in some areas (mainly to the north-west of Razgrad) there is a particular coloration of concentric light brown, reddish and grayish circles. The size of the nodules is 5–20 cm long, less often up to 60 cm in length (Fig. 3). The surface of the flint at the break is smooth, less often conchoidal; gray concretions are distinguished by a coarser break. These features, with the smooth surface and regular ellipsoidal shape, are diagnostic of Ludogorian flint. Its mineral composition mainly includes cryptocrystalline and microcrystalline chalcedony, morganite, and quartz. All bio components are silicified

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Fig. 2 Lower Cretaceous Aptian (Ludogorian) flint: 1—flint nodule, regular ellipsoidal shape, and thick calcareous crust (8–12 mm). Locality “Chukata,” north of the town of Razgrad. Sample No. 1434 of the collection of the Museum “Earth and People” (Nachev 2009); 2—flint nodule (1/4 part), beige and dark yellow patina, formed in the aquatic environment. The village of Ravno, south of the city of Kubrat. Sample No. 1438 from the collection of the Museum “Earth and People” (Nachev 2009)

and consist of, as a rule, spicules and, more rarely, fragments of foraminifera and dinoflagellates (Nachev 2009). The locations of this type of flint, studied by Nachev and Kanchev (1984), could be classified as secondary deposits: eluvial (originated at the place of primary deposits as a result of the washing out of chalky rocks with water) and palaeoalluvial (accumulations of nodules resulting from the flow of ancient rivers). These secondary deposits appeared as a result of the erosion of the primary deposits (Nachev and Kunchev 1984). Aptian flint redeposited in the Quaternary period was used during the Chalcolithic. To the day, the following workshops for its primary processing have been documented: Chukata, Nedoklan, Dryanovets (near the town of Razgrad), Topchii, Kamenovo-Ravno (near the town of Kubrat), Chakmaka (near the town of Isperih), Kriva Reka (near the city of Shumen) (Kanchev et al. 1981; Skakun 1984, 1993, 1999; Mateva 2009, 2011; Zidarov et al. 2016; Boyadzhiev et al. 2020). Flint mining was carried out in shallow pits without reaching into the thickness of the chalky rocks since the highest quality raw materials were under the loess cover in dense interlayers within the weathered layers of Aptian chalk (Fig. 4). Nodules from these localities do not have inclusions and cracks. Still, they are large, which allows splitting them only with the help of new lever method of knapping that occurred during the Chalcolithic. It also allowed for the improvement of the previously known methods of flint processing to obtain correct, technically optimal blanks for tools—macroblades of considerable length (Skakun 1984, 1999, 2006; Pelegrin 2002; Skakun et al. 2017). A deposit where the primary processing of flint from the eluvial deposit was carried out in the Chalcolithic is located south-west of the settlement of Ravno (see Fig. 1). Kanchev, when examining this territory, observed two accumulations of flint-working

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Fig. 3 Pre-cores from the Chakmak tell, Isperikh district (left) and nodule from the Kamenovo tell, Kubrat district (right). Scale—60 cm (Mateva 2009)

wastes—Ravno I and Ravno II. Still, due to the lack of pottery, he considered them as Paleolithic workshops (Kanchev 1985). A more thorough study (Mateva 2009) suggested that an area of about 100 hectares, designated by Kanchev as Ravno II, was an accumulation of cores and the waste of their knapping, reaching a thickness of 1.5 m. The presence of cores typical to the Chalcolithic is a clear marker of the existence of a huge flint-working workshop. The absence of ceramics and household finds can be explained by the fact that the craftspeople worked in the workshop during the day but lived in the settlement at the Kamenevo Tell, which was 4 km away from the workshop (Manolakakis 2011). Similar workshops for the primary processing of flint existed in Izbegli (Bulgaria, the Plovdiv region) and Kriva Reka before it was destroyed by medieval and modern industrial flint mining. The ancient mining and primary flint processing site near the village of Tetovo, Ruse region, was also destroyed by a modern limestone quarry (Stojanova and Kunchev 1984). Archaeological studies confirm that during the Chalcolithic, flint was exploited from the weathered layer of the pits; the deeper layers began to be exploited in the later periods only after the exhaustion of the overlying deposits. Workshops for flint tools manufacturing were also discovered in north-eastern Bulgaria. Two such findspots have been partially explored: the Kamenovo Tell (Late Chalcolithic, near the city of Kubrat) (Boyadzhiev et al. 2020) and the Chakmaka Tell (Middle Chalcolithic, near the city of Isperih). During the excavations at the Kamenovo Tell, a significant number of blade blanks for the manufacture of various tools were found, as well as a workshop for the production of flint axes and

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Fig. 4 The occurrence of Ludogorian flint in the thickness of the chalk. Tetovo quarry, the Ruse region (Mateva 2009)

adzes (Manolakakis 2011). During the excavations of the Chalcolithic burial ground, located near the tell, a large number of flint finds were discovered. According to the authors of the excavations, after the burial ground was abandoned, activity associated with flint processing took place in the site’s area (Boyadzhiev et al. 2019). Further excavations and comprehensive studies of the materials obtained will make it possible to clarify whether it was a workshop or just a waste dump. Even if it turns out to be a dump of production waste, then, without doubt, it comes from a workshop undetected so far on the tell itself or outside it (Boyadzhiev et al. 2020). The Chakmaka Tell in the Isperih district is located 1.5 km from a small but easily accessible palaeoalluvial flint outcrop in a ravine on the right bank of the Sazlaka River, which today is a small stream. In addition to the flint outcrops, accessible even today, on the river terrace and along the slopes of the ravine, there are remains of a workshop for the primary processing of raw materials. There are not many finds of flint concretions on the tell. Still, the flint inventory of the settlement presents all stages of processing of the raw materials: more than a hundred pre-cores and cores, hundreds of lamellar blanks, and fully formed tools. Their location in the interhouse space layer coincides with ethnographic (Shkorpil and Shkorpil 1892, 1898) and archaeological (Tsvek and Movchan 2005) data on identifying flint processing workshops in residential settlements, where professional craftspeople were engaged in the manufacture of various high-quality tools. The main knapping method was the pressure technique, while large long blades were obtained using new technology, namely, the enhanced pressure with the help of a lever device. High-quality products

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indicate that the flint was processed by professional craftspeople (Skakun 1999; Pelegrin 2002). The results of the technical and morphological study of the flint inventory of the Chalcolithic settlements located in different regions of Bulgaria and Romania show that its distinguishing feature is the stable unification of flint products. The production inventories of the settlements of Ruse (Early to Late Chalcolithic); GolyamoDelchevo (Early to Late Chalcolithic); Polyanitsa (Early to Middle Chalcolithic); Provadiya-Solnitsata (Early to Middle Chalcolithic); Ovcharovo (Middle to Late Chalcolithic); Kosharna (Late Chalcolithic); Demir baba teke (Late Chalcolithic); Sredoseltsi (Late Chalcolithic); Durankulak (Late Chalcolithic); Kojadermen (Late Chalcolithic); Sushina (Late Chalcolithic); Vinitsa (Late Chalcolithic); Hotnitsa (Late Chalcolithic); Yunatsite (Late Chalcolithic); Kazanlak (Late Chalcolithic); Dyadovo (Late Chalcolithic); Dolnoslav (Late Chalcolithic); Pietrele (Late Chalcolithic); Mariutza (Late Chalcolithic); the Kosharna necropolis (Late Chalcolithic); the Varna necropolis (Late Chalcolithic); the Durankulak necropolis (Late Chalcolithic) have direct analogies in terms of the type of flint raw material and the technical and morphological characteristics of tools with those from the workshop settlements—at Kamenevo, Chakmaka I, etc. The common feature is the main types of blanks—fragments of regular blades and most typologically distinct tools: endscrapers on blades, angled burins on blade fragments, drills with a triangular point, notched blades, retouched blades, etc. The main difference, as use-wear studies show, is that most of these tools from the workshop settlements do not have use-related traces, while tools from consumer settlements, as a rule, have traces of use indicating various functions. The uniformity of the blanks and the main types of tools, as well as the absence of the Ludogorian cores and flint-working wastes in the consumer settlements, indicate the imported nature of the flint tools, which were products of the flint workshops at Ludogorie. These observations indicate that the settlements farther away from the Ludogorian flint deposits received no raw materials, only finished products in the form of blades and their fragments (Skakun 2006). Their standard character led to a distinct series of tools, among which the frequency of random or transitional forms is insignificant. The most remote Bulgarian consumer settlements of Ludogorian flint products are located 100–150 km from the producing centers. The distance to the Romanian workshop-tells at Pietrele and Mariutsa (Late Chalcolithic) is about 180 km (Mateva and Parnic 2011; Gatsov and Nedelcheva 2019; Gurova 2019). Products from Ludogorian raw materials were also found at the sites of the Bolgrad-Aldeni II and Tripolye cultures in Ukraine (Skakun 1986). At the end of the Late Chalcolithic, at settlements (Mariutsa, Hotnitsa, and Sushina) more distant from the centers of mining and primary processing, there are signs of a certain lack of raw materials, expressed in their more economical use and the presence of a larger number of combined and reused tools. Thus, the studies demonstrate not only the high technique of extraction and processing of Ludogorian flint, the complex organization of flint-working production but also stable industrial relations, which made it possible to provide a large number of consumers with the necessary tools.

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4 Conclusions The research testifies to the occurrence and functioning of the large-scale exploitation of Ludogorian flint during the Chalcolithic in the northeast of Bulgaria. A number of specific features characterize the structure of the flint-working production at that time. Among them is the presence of workshops for the primary processing of flint located near its deposits and the functioning of large specialized workshops on the territories of nearby settlements. Indisputable proof of supplies of Ludogorian blanks and tools from the single production centers of the north-eastern part of Bulgaria to the settlements-consumers are the following facts: the unity of flint raw materials, the unity of the flint knapping technology, and, as a result, the uniformity of the blank types and most types of basic tools. These data indicate the great achievements of both the flint industry and the high degree of economy development and economic ties that existed during the Chalcolithic in this part of south-eastern Europe. Acknowledgements The development of a comprehensive methodology of experimentaltraceological analysis (FMZF-2022-0012 “The oldest inhabitants of the North of Eurasia: human settlement in the Stone Age, production technologies”).

References Bibikov, S.N.: On the early forms of craft production. In: Domashnie promisli i remeslo [Home production and crafts]. Leningrad, pp. 3–6 (1970) (in Russian) Boyadzhiev, Y., Chernakov, D., Dilov, D., Guadeli, A.: Chalcolithic necropolis, and flint production center in the village of Kamenovo, Razgrad region. Arheologicheski otkritia i razkopki prez 2019 g. [Archaeological discoveries and excavations in 2019], vol. 1, pp. 307–310 (2019) (in Bulgarian) Boyadzhiev, Y., Skakun, N., Chernakov, D., Terekhina, V., Gatsov, I., Nedelcheva, P.: New data on the prehistoric flint workshop near the village of Kamenovo, NE Bulgaria. Izvestia Na Natsionalnia Istoricheski Muzey [proceedings of National Historical Museum] 31, 46–58 (2020). (in Bulgarian) Coms, a, E.: Les matières premières en usage chez les hommes néolithiques de l’actuel territoire Roumain. Acta Archaelogica Carpathica 16, 239–249 (1976) Gatsov, I., Nedelcheva, P.: Pietrele: Lithic Industry. Finds from the Upper Occupation Layers. Herbert-Verlag. Bonn, 86p. (2019) Gurova, M.: Book review: Ivan Gatsov and Petranka Nedelcheva. Pietrele 2: Lithic industry. Finds from the Upper Occupation Layers. Bonn: Habelt-Verlag, 2019. Bulgarian e-J. Archaeol. 10(1), 149–156 (2020) Kanchev, K.: Flint rocks in Bulgaria and their use. Arkhiv AIM BAN [Archive of NAIM BAS]. Sofia (1985) (in Bulgarian) Kanchev, K., Nachev, I., Kovnurko, G.: Flint rocks in Bulgaria and their exploitation. Interdistsiplinarni Izsledvania [interdisciplinary Studies] 7–8, 41–59 (1981). (in Bulgarian) Manolakakis, L.: A flint deposit, a tell and a shaft & A lithic production complex Ravno3-Kamenovo? (Early Chalcolithic, North Eastrn Bulgaria). Studia Praehistorica 14, 225–214 (2011)

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Mateva, B.: About of the organization of the primary processing of flint in the Eneolithic (geological data and ethnographic parallels). In: S.N. Bibikov I pervobitnaia arheologia [S.N. Bibikov and primeval archeology]. St.-Petersburg, pp. 350–355 (2009) (in Russian) Mateva, B.: Exploiting of flint deposits in north-eastern Bulgaria in Chalkolith. In: The Lower Danube in prehistory: landscape changes and human-environment interactions, Proceedings of the International Conference Alexandria, 3–5 November 2010, Bucure¸sti, pp. 173–179 (2011) Mateva, B.: Functional analysis of flint tools from the upper layer of the tell Hotnitsa (in print 2021) (in Bulgarian) Mateva, B., Parnic, V.: Typological and use-wear analysis of flint tools from Tell M˘ariut, a, jude¸tul C˘al˘ara¸si. Orient S, i Occident, Cultur˘a Si ¸ Civiliza¸tie La Dun˘area De Jos 28, 116–127 (2011) Nachev, C.: The basic flint types as raw material for flint tools production. Interdistsiplinarni Izsledvania [interdisciplinary Studies] 20–21, 7–22 (2009). (in Bulgarian) Nachev, I., Nachev, Ch.: Distribution and evolution of siliceous rocks in Bulgaria. In: Hein J.R., Obradovich J. (ed.). Siliceous deposits of the Tethys and Pacific Regions, pp. 81–92. New York. Berlin, Heidelberg (1989) Nachev, I., Kunchev, K.: Aptian and quaternary flint in North-East Bulgaria. In: III-d Seminar on Petroarchaeology. Reports. Plovdiv, pp. 65–82 (1984) Pelegrin, J.: La production des grandes lames de silex du Grand-Prissingy. In: Matériaux, production circulation, du Néolithique à l’âge du Bronze. Paris, pp. 131–147 (2002) Popov, R.: Culture and life of prehistoric man in Bulgaria 1 (Stone Age). Sofia, 60p. (1928) (in Bulgarian) Shkorpil, K., Shkorpil, V.H.: Northeastern Bulgaria in geographical and archaeological attitude]. Sbornik za narodni umotvorenia, nauka i knijnina. Collection of folk tales, science and literature, vol. 7, pp. 3–83 (1892) (in Bulgarian) Shkorpil, K., Shkorpil, V.H.: Telles. Sofia, 176p. (1898) (in Bulgarian) Skakun, N.N.: Flintworks in the paleometal age in Bulgaria. In: III-d Seminar on petroarchaeology. Reports. Plovdiv, pp. 83–92 (1984) (in Russian) Skakun, N.N.: Tools and economy of the Bolgrad (Aldeni II) Eneolithic culture. Studia Praehistorica 8, 91–107 (1986). (in Russian) Skakun, N.: The development of the production in the Early Metal epoch in Bulgaria. Pulpudeva 6, 152–164 (1993). (in Russian) Skakun, N.N.: Progress of technology in the Chalcolithic in the South-East of Europe: (Based on the materials of agricultural cultures in Bulgaria). Arheologicheskie Vesti [archaeological News] 6, 287–307 (1999). (in Russian) Skakun, N.N.: Tools and economy of the ancient agricultural tribes of South-Eastern Europe in the Eneolithic (based on the materials of the Varna culture). Trudy IIMK RAN [Proceedings of IHMC RAS] 21. Publishing house “Nestor-History”. St.-Petersburg, 224p. (2006) (in Russian) Stojanova, V., Kunchev, K.S.: Exploitation of the silleceous rocks from Izbegli deport (Plovdiv district). In: III-d Seminar of petroarchaeology.Reports. Plovdiv, pp. 282–300(1984) Todorova, H.: Stone copper age in Bulgaria. Publishing house “Nauka i izkustvo”. Sofia, 278p. (1986) (in Bulgarian) Tzvek,E. Movchan, I.: Chalcolithic manufacturing complex for the flint extraction and processing on the BolshayaVys River, Ukraine]. In:Na poshanuSofiiStanislavivniBerezans’koi[In memoriam Sofia Stanislavovna Berezanskaya]. Kyiv, pp. 66–76 (2005) (in Russian) Skakun, N., Mateva, B., Terekhina, V.: Production, and use of long blades during the Chalcolithic in North-Eastern Bulgaria. Cuadernos De Prehistoria y Arqueología De La Universidad De Granada 27, 141–165 (2017) Zidarov, P., Mateva, B., Gurova, M., Dilov, D.: Chalcolithic workshops for flint production in Ludogorie: non-destructive researchs at Lavino-Chakmaka and Kamenovo-DuzOrman sites, Razgrad region. Arheologicheski otkritia razkopki prez 2016 g. [Archaeological discoveries and excavations in 2016], vol. 1, pp. 729–731 (2017) (in Bulgarian)

Geochemical Data on the North-Western Caucasus Chert Sources and Origin of the Middle Palaeolithic Artifacts Ekaterina V. Doronicheva, Marianna A. Kulkova, and Vladimir A. Tselmovitch

Abstract Identifying the sources of origin of lithic raw materials is crucial for addressing hominid mobility patterns and adaptations in the Paleolithic. Among the raw materials exploited in the past, the most commonly used lithic raw material in the Palaeolithic of Europe and the Caucasus was chert (flint). With few exclusions, Eastern-European archaeology lacks a complex systematic study of raw material strategies, including surveying and sampling chert (flint) sources, serial geochemical and petrographic analyses of samples from sources and Middle Palaeolithic sites. The authors report results of geochemical analyses of chert (flint) sources, discovered and sampled in the North-Western Caucasus, which were studied using several methods. XRF analysis has been performed on 98 geological samples from chert outcrops, including samples from 9 different chert-bearing geological strata from 21 outcrops in the region. Additionally, scanning electron microscopy was performed on 15 samples from these outcrops and 23 chert artifacts by SEM and nine samples by XRF from Middle Palaeolithic sites in the region, including Mezmaiskaya cave, Hadjoh-2, and Besleneevskaya open-air sites, dated from 70k–80k to 40k BP were studied. Keywords Lithic raw material procurement · Geochemistry · XRF analysis · SEM · North Caucasus · Middle Palaeolithic

E. V. Doronicheva (B) Laboratory of Prehistory, Saint Petersburg, Russia e-mail: [email protected] M. A. Kulkova Herzen State Pedagogical University, Saint Petersburg, Russia V. A. Tselmovitch Schmidt Institute of the Physics of the Earth RAS, The “Borok Geophysical Observatory” Branch, Borok, Russia © The Author(s), under exclusive license to Springer Nature Switzerland AG 2023 N. N. Ankusheva et al. (eds.), Geoarchaeology and Archaeological Mineralogy—2021, Springer Proceedings in Earth and Environmental Sciences, https://doi.org/10.1007/978-3-031-16544-3_10

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1 Introduction Lithic raw material analysis and characterization are essential for Paleolithic archaeology, helping to understand human adaptations and mobility. Chert (flint) was one of the most commonly used raw materials for making tools in the Palaeolithic of Eurasia, including the Caucasus. The origin of chert artifacts was previously defined based on petrographic analyses of samples from geological outcrops and archaeological sites (e.g., Grégoire 2000; Doronicheva et al. 2016). In the last 15 years, geochemical analyses have been commonly used (e.g., Malyk-Selivanova et al. 1998; Moreau et al. 2016, 2019; Brandl et al. 2018; Sánchez de la Torre et al. 2017, 2020). In 2007, studies on Paleolithic lithic raw materials began in the NW Caucasus. These studies include surveying for chert (flint) outcrops and studying petrographic characteristics of chert samples and artifacts (Doronicheva et al. 2012, 2016). However, geochemical data on regional chert (flint) sources have not been analyzed yet. For the first time, this paper reports preliminary results of geochemical research of chert samples from both geological outcrops and the Middle Palaeolithic (MP) sites in the region. Our research is based on two geochemical methods: X-ray fluorescence (XRF) analysis and scanning electron microscopy (SEM). In the NW Caucasus, most MP sites show the development of a local variant of the Eastern Micoquian industry between approximately 90k and 40k BP (Fig. 1; Golovanova and Doronichev, 2003). Three major stages of the Eastern Micoquian Neanderthal occupation of the region are defined (Golovanova 2015). Our previous research on lithic raw material originating from the Eastern Mocoquian region has shown (Doronicheva et al. 2016) that local Neanderthals actively exploited local and non-local flint sources. The range of exploited sources varied in different stages of the MP (Fig. 1a–c).

2 Materials and Methods Since 2007, one of us (ED) has been creating a reference collection of lithic raw material source standards (lithotheque) of mainly siliceous rocks from outcrops in the Northern Caucasus. Now it consists of more than 1000 samples from 60 outcrops and is stored in the Laboratory of Prehistory in St.-Petersburg, Russia. Our previous research (Doronicheva et al. 2012, 2016) indicated that the NW Caucasus primary chert outcrops are mainly related to limestones of the OxfordKimmeridgian stratum of the Upper Jurassic epoch. These includes such sites as Azish-Tau (KR-1), Unakoz (KR-2), Berezovaya Balka (KR-12), Rufabgo (KR-32– 33), Gamovskaya balka (KR-34), Meshoko (KR-47), and many others. Chert of grey and brown colors prevail. In contrast, in the Besleneevskaya (KR-3–5) and Shedok (KR-23) flint outcrops dated to the Cretaceous period of the Senonian epoch, various colored flints (red, honey, and other colors) are present. The Senonian flints differ

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.Fig. 1 Map showing Eastern Micoquian sites in the Northwestern Caucasus and chert sources exploited in different periods of the Middle Palaeolithic. The red star marks the Zayukovo (Baksan) obsidian source. The black ellipse marks the distribution area of the chert sources used in the Mezmaiskaya cave. a Sites: 1—Mezmaiskaya, 2–3—Hadjoh-2 and SredniyKhadjoh, 4—Il’skaya I and II. Flint sources (geological outcrops): 1—Azish-Tau (KR-1), 2—Unakozovskoye-1 (KR2), 3—Shahan-2–4 (KR-9–10), 4—Meshoko (KR-47), 5—Gubs (KR-7–8), 6—BesleneevskayaI and II (KR-3–5), 7—Shedok (KR-23), 8—Akhmet-Kaya-2, and 3 (KR 42–44), 9—alluvial flint sources near Il’skaya I and II sites, 10—Lysogorka (300 km from Mezmaiskaya). b Sites: 1—Mezmaiskaya, 2—Hadjoh-2, 3–4—Barakaevskaya and Monasheskaya. Flint sources: 1— KR-1, 2—Shahan-2–4 (KR-9–10), 3—Meshoko (KR-47), 4—KR-3–5, 5—KR-7–8. c Sites: 1— Mezmaiskaya, 2—Matuzka, 3—Hadjoh-2, 4–6—Monasheskaya, Gubsrockshelter 1, Autlevskaya cave, 7—Besleneevskaya-1, 8—Baranakha-4. Flint sources: 1—KR-1, 2—KR-2, 3—Shahan-1– 4 (KR-6 and 9–10), 4—KR-47, 5—KR-3–5, 6—KR-7–8, 7—KR 42–44, 8—Berezovaya Balka (KR-12), 9—Baranakha (KR-14), 10—Lysogorka

from the Upper Jurassic cherts in a general texture and a lower frequency of mineral and organic inclusions. Petrographic and geochemical analyses were performed on samples collected from different parts of the chert-bearing outcrops analyzed. Petrographic descriptions were previously published by Doronicheva et al. (2012, 2016). The compositions of chemicals and trace elements in samples were determined by XRF analysis using a Spectroscan MAX device. The data shows the concentration of chemical elements, such as V, Cr, Fe, Co, Ni, Cu, Zn, Sr, Pb, Rb, Ba, La, Y, Zr, Nb, and As, as well as oxides, such as TiO2 , MnO, CaO, Al2 O3 , SiO2 , P2 O5 , K2 O, MgO, Na2 O in percentage by weight. This analysis is one of the most effective methods used for the elemental analysis of chemicals because it provides complete and reliable information on the elemental composition of samples in a minimal time. Additionally, we applied SEM using a TESCAN VEGA II scanning electron microscope and X-ray microanalyses techniques, such as energy-dispersive X-ray spectroscopy (EDS) and wavelength-dispersive X-ray spectroscopy (WDS) using Oxford Instruments’ EDS and WDS spectrometers. With the help of SEM and X-ray microanalysis, the mineral composition of impurities and some fine structural and textural features have been defined for samples, allowing better distinguish textural features characteristic of each flint-bearing geological deposit. The EDS and WDS spectra were processed using the INCA software package (Oxford Instrument Analytical Ltd.). For the current study, we used archaeological artifacts sampled from four stratified MP sites in the region: Mezmaiskaya and Matuzka cave sites, and Hadjoh-2 and Besleneevskaya sites (see Fig. 1). To identify groups of samples from geological outcrops and artifacts from sites that are characterized by a similar composition of chemical elements and originate from the same type of geological deposit, the data obtained using XRF were processed by methods mathematical statistics.

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3 Results and Discussion In the plot obtained using principal component analysis (PCA) (Fig. 2a), only the chemical elements which average fraction exceeded 0.01% in the sample composition (see Table 1) were taken into account. PC I and PC II together cover about 50% of the total variability in the chemical composition of the samples. PC I differentiates the samples mainly by the content of CaO, Na2 O, and SiO2 . In samples with relatively low silica content, proportions of CaO and Na2 O are usually larger. Although PC I does not differentiate samples from different geological outcrops by these chemical elements, it shows that KR-3–5, KR-32–33, and KR-12 have also reduced SiO2 content. Among the samples analyzed from archaeological sites, samples 1 and 2 from Hadjoh-2 demonstrate a similar relationship, while samples 7 and 8 from layer 2a at Mezmaiskaya show a reverse tendency. PC II delimits the samples by the content of Fe, Ba, CaO, Al2 O3 , K2 O, but, like PC I, PC II does not differentiate samples from different outcrops by these chemical elements. PC II indicates that in the samples with a high content of CaO, the proportion of other elements is lower than in the samples with a high proportion of CaO. Again, samples 1 and 2 from Hadjoh-2 characterized by a high content of CaO are distinguished, whereas sample 5 from layer 3 at Mezmaiskaya falls on the opposite end of the range for this component. Also, PC II shows that samples from KR-1 and KR-32–33 chert sources differ from samples KR-9–10 by a higher value of CaO and the lower values of Fe, Ba, Al2 O3 , and K2 O. The SiO2 boxplot (Fig. 2b) indicates that two main groups of geological samples can be identified. The first group, characterized by high (>95%) values of SiO2 , includes Gubs (KR-7–8), Shedok (KR-23), Akhmet-Kaya (KR-42–44), Besleneevskaya (KR-3–5), Shahan (KR-9–10) and Azish-Tau (KR-1) sources (with some outliers) that are related to both the Oxford-Kimmeridgian and Senonian strata. The second group, characterized by the lower (