Phosphate Analysis

The properties of porous hydroxyapatite (HA) bioceramic produced by heat treatment (annealing) of bovine bone were evaluated over temperatures between 400 T and 1200 T. The annealed body was characterized by thermal analysis (thermogravimetric analysis (TG)/differential thermal analysis (DTA)), scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX) and Fourier transformed infrared (FTIR) spectroscopy. The XRD results showed that the annealing process enhanced the crystallinity of HA phase in the bone matrix particularly when annealed above 700 degrees C. There was no secondary phase formation in bones annealed between 600 degrees C and 1000 T. However, decomposition of HA to P-tricalcium phosphate (TCP) was observed for samples heat-treated at 1100 degrees C and 1200 degrees C. The FTIR spectra and the TG/DTA thermogram of as-received bovine bone indicated the presence of organic compounds, which upon annealing at temperatures above 600 T was completely removed from the matrices. Bovine bone annealed between 800 degrees C and 1000 degrees C revealed the characteristics of a natural bone with the interconnecting pore network being retained in the structure.

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A new crystallinity index (CI), based on the X-ray powder diffractometric pattern of fossil bone carbonate hydroxylapatite, is defined. This CI value provides a semi-quantitative way to estimate the diagenetic changes in archaeological and palaeontological bone phosphate. The studied samples are 71 human bones from the French merovingian cemetery of Saint-Linaire (1200-1700 ), 37 human bones from two necropoleis in Niger (1000-5000 ), two cave bear bones from Aldène Cave (southern France; around 70,000 ), five bones of Miocene mammals and 14 bones of Mesozoic reptiles. The main results are that: (1) there is no correlation between the increase in the CI and the age of the sample, even in one given locality; (2) the CI seems to be related to the taphonomical conditions, in archaeological and fossil bones; (3) an increase in the CI is correlated with a loss in organic matter in one archaeological site, but the quality of preservation of organic matter in fossil bones does not depend on the changes in the CI; (4) the correlation between the increase in the CI and the decrease of CO 3 amount in bones from the Niger necropolies suggests a possible mechanism for the increase in crystallinity. The changes of crystallinity reflect early diagenetic changes and depend on the burial environments.

The sinterability of nanocrystalline hydroxyapatite (HA) particles by microwave sintering was compared with conventional pressureless sintering. The results revealed that microwave heating was effective in producing a useful HA body in a very short sintering cycle without disrupting the HA phase stability. The maximum hardness of 7.21GPa and 6.38GPa was obtained ford HA sintered at 1050 degrees C by the conventional method and 1150 degrees C by microwave sintering, respectively. The maximum fracture toughness measured for the microwave-sintered and conventional-sintered HA was 1.45 MPam(1/2) at 1050 degrees C and 1.22 MPam(1/2) at 1000 degrees C, respectively. Although the relative density of microwave -sintered HA was slightly lower than the conventional - sintered HA throughout the sintering regime employed, taking into account of the heating and soaking periods, the time taken by microwave sintering to achieve a relative density of 96.5% was about 3% of the time consumed for samples sintered by the conventional heating. Microwave heating was found to be an effective technique to produce a useful HA body for clinical applications without causing grain coarsening.


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The study of archaeological sediments is an important source of information on how humans lived at a site. Attributes of human site use such as frequency of visits and duration of stay can be explored by measuring changes in phosphorus (determined using X-ray fluorescence) and carbon concentrations in sediments and magnetic susceptibility of sediments in combination with analysis of other sediment attributes, stone artefacts and faunal remains. This study concludes that increases in phosphorus and carbon concentrations and the discard rate of stone artefacts at Marillana A rockshelter in the inland Pilbara, Western Australia, indicate an increase in the frequency of site use with no change in the function of the site. This is interpreted as representative of an increase in regional population density.

In this report, we demonstrate that continuous improvement in XPS instruments and the calibration standards as well as analysis with standard component-fitting procedures can be used to determine the binding energies of compounds containing phosphorus and sulfur of different oxidation states with higher confidence. Based on such improved XPS analyses, the binding energies (BEs) of S2p signals for sulfur of increasing oxidation state are determined to be 166-167.5 eV for S=O in dimethyl sulfoxide, 168.1 eV for S=O 2 in polysulfone, 168.4 eV for SO 3 in polystyrene sulfonate and 168.8 eV for SO 4 in chondroitin sulfate. The BEs of P2p signals show the following values: 132.9 eV for PO 3 in triisopropyl phosphite, 133.3 eV for PO 4 in glycerol phosphate, 133.5 eV for PO 4 in sodium tripolyphosphate and 134.0 eV for PO 4 in sodium hexametaphosphate. These results showed that there are only small increases in the binding energy when additional oxygen atoms are added to the SO chemical group. A similar result is obtained when the fourth oxygen or poly-phosphate environment is added to the phosphorus compound. These BE values are useful to researchers involved in identifying oxidation states of phosphorus and sulfur atoms commonly observed on modified surfaces and interfaces found in applications such as biomaterials, super-capacitors and catalysis.

Data on phosphatase activity (PA) in soils of different natural zones, intrazonal soils, buried soils, and cultural layers in archaeological monuments of different age were summarized. The variability of PA in soil complexes was analyzed. The maximum values of PA were recorded in the upper horizon of Eutric Reti-sols, and minimum values were found in Haplic Calcisols of the Baer hills in the Caspian Lowland. In Solo-netzes, a wider variation of PA in the A1 horizon was recorded as compared to that in Cambisols and Calci-sols. Mean value of PA in the upper horizon of Solonetz was 1.5 times higher than in the upper horizon of Cambisols and Calcisols. The maximum values of PA in the profile of Solonetz were determined in the uppermost 2-cm-thick layer. The B1 horizon of Cambisols and Calcisols had a higher PA in comparison with that in the A1 horizon of these soils, whereas the B1 horizon of Solonetz had a lower PA than that in the A1 horizon. In the paleosols buried under kurgans of different age, PA was higher in paleosols buried in humid epochs than in paleosols buried in arid epochs. Cultural layers of ancient settlements had the maximum variability of PA values. In some cases, in the cultural layers with low organic matter content, the values of PA correlated with the content of phosphates. In the cultural layers with ash and charcoals, the low values of PA were recorded at high phosphate content.

This paper presents the results of phosphorus mapping conducted on a number of coastal activity zones on the multi-period, archaeological farm site of Vatnsfjörður, northwest Iceland. The aim of the study was to detect the exact levels and extents of shorelines contemporary with the archaeological site's activities and to use sea-level change to establish a relative chronology of coastal activity zones. Absolute dating of the coastal zones and sea-level changes was achieved by integrating an existing sea-level curve with a novel tephrochronology-based curve, created for the purpose of this research. Results were projected onto a detailed digital terrain model of the area in order to reconstruct the extent of the coastline contemporary with human activity in the respective zones. A significant component of the research was an attempt to develop the existing approach to phosphorus mapping results interpretation. This has resulted in an improved methodology that can be applied to the dynamic and challenging environments of coastal sites worldwide.

The here presented PhD project explores the phenomenon of cereal cultivation during the Iron Age (c. 500 BC – AD 1100) in southern Scandinavia. The main body of the thesis consists of four articles. These were written with the aim to identify chronological, geographical, theoretical and methodological gaps in current research, to develop, apply and evaluate approaches to how new knowledge on Iron Age cereal cultivation can be attained, and to assess the interaction between archaeobotany and other specialisms currently used in settlement archaeology. The introduction section of the thesis also contains a historical overview of archaeobotanical research on cereal cultivation in southern Scandinavia.

The first article is a compilation and summary of all available previously performed  archaeobotanical investigations in southern Sweden. This data is compared and discussed in relation to similar publications in Denmark and smaller scale compilations previously published in Sweden. The main result of the study is an updated and enhanced understanding of the main developments in the investigation area and a deepened knowledge of local development chronologies and trajectories in different parts of southern Sweden.

The second article is a methodological presentation of a multiproxy analysis combining plant macrofossil analysis, phosphate analysis, magnetic susceptibility analysis and measurement of soil organic matter by loss on ignition. The applicability of the method for identification and delineation of space functions on southern Scandinavian Iron Age sites is discussed and illustrated by two case studies from the Danish site of Gedved Vest. Particular focus is placed on exploration of the use of the functional analysis for assessment of taphonomic and operational contexts of carbonised plant macrofossil assemblages.

The third article aims at presenting an Iron Age cereal cultivation history for east-central Jutland, an area identified at the outset of the project as under-represented in archaeobotanical studies. The article combines data from depth analyses of material from the sites of Gedved Vest and Kristinebjerg Øst (analysed with the methods and theory presented in the second article) with a compilation of previously performed archaeobotanical analyses from east-central Jutland. The main results of the study are that developments in the study area appear to follow a chronology similar to that previously observed on Funen rather than the rest of the peninsula. Rye cultivation is furthermore discussed as more dynamic and flexible than previously presented in Scandinavian archaeobotanical literature.

The fourth and final article leaves archaeobotany as the main topic. It focuses instead on evaluating, theorising and expanding the multiproxy method presented in the second article by a thorough comparison of the botanical, geochemical and geophysical methods to other techniques of functional analysis currently used in archaeology. These techniques include studies of artefact distributions, assessments of spatial relations between settlement features, and studies of the structural details of dwellings and other constructions. The main result is that there is a correspondence between the functional indications provided by botanical, geochemical and geophysical methods and techniques used in mainstream archaeology. The comparison furthermore shows that a combination of the two data sets allows for more highly resolved functional interpretations than if they are used separately.

The main conclusion of the PhD thesis, based on the discussions in all four articles, is that archaeobotanical questions commonly necessitate the assessment of non-botanical archaeological material. The comparison of archaeobotanical data to other segments of the archaeological record does, however, enable the use of the former as an archaeological resource for addressing non-botanical questions. The increased understanding of (mainly settlement) site dynamics resulting from this integration of methods allows archaeobotanists to address increasingly complex botanical questions. Increased and more structured integration between archaeobotany and other specialisms operating within the framework of settlement archaeology is therefore argued to be the preferred approach to performing both high quality archaeobotany and settlement archaeology.

Many reconstructions and models of the Late Prehistoric period in the Ohio Valley discuss changes in the structure and organization of primary habitations. These changes are often associated with changes in social organization, intra-community relationships, and socio-political complexity. It is also being increasingly recognized that typological Culture Historical narratives often over-simplify or misconstrue actual local trajectories. What is needed to both develop accurate historical narratives and test extant models is a very large sample of communities with a reconstructed organization pattern. Excavation is not an efficient way to increase the size of the known sample of community organization patterns; however, excavation is still the dominant method of archaeological investigation in the region.

In this dissertation I illustrate a multi-staged approach to quickly reconstruct the structure of a given archaeological site (irrespective of time period) applied specifically to a Late Prehistoric community in the Middle Scioto Valley: the Reinhardt Village (33PI880). The approach used here begins with a suite of minimally invasive/destructive data-generation techniques (extensive surface survey, intensive surface survey, volumetric shovel testing, gradiometry, magnetic susceptibility, and soil phosphate) supplemented by excavation. The minimally invasive techniques provided most of the salient details regarding settlement structure and if employed iteratively in a regional survey could quickly increase the database to reconstruct local prehistory and test extant models. Specifically, the strategy employed at Reinhardt could be used to reconstruct 2 – 4 community structures in the typical field school, summer season.

The results at the Reinhardt site reveal a small, late fourteenth century planned community. The Reinhardt community is organized around an open, oblong plaza oriented northeast-southwest with multiple activity areas roughly concentrically around the plaza. The Reinhardt community varies from a typical plan in that the activity zones are irregularly distributed around the plaza, with an isolated productive area south and outside of the concentric zones. The Reinhardt investigations add to the knowledge of variability of community structure for the Middle Ohio River Valley in general, but specifically for the Middle Late Prehistoric period of the Scioto River Valley.

Radoslaw Grabowski 2014. Identification and delineation of settlement space functions in the South Scandinavian Iron Age: Theoretical perspectives and practical approaches This article presents an overview of methods used in south Scandinavian archaeology for identification and delineation of settlement space functions. The overview includes commonly utilised archaeological approaches, such as artefact distribution studies and inferences based on assessment of house and settlement morphologies, as well as archaeobotanical, geochemical and geophysical approaches to functional analysis. The theoretical potential and limitations of each presented functional parameter are outlined and thereafter applied and compared using material from five case study sites in east-central Jutland, Halland and Bohuslän. The presentation of the site of Gedved Vest in east-central Jutland also incorporates a comparison of two common approaches to geochemical sampling: 1) sampling and analysis of soil retrieved from feature fills, and 2) horizontal sampling of soil from the interface between the topsoil (A/ Ap) and the subsoil (C) -horizons along a pre-determined grid.

Snowdonia has hundreds of Bronze Age burial cairns, of a wide variety of types, of which some 50 are located on mountain-tops between 500 and 1100m above sea level. The excavations at Drosgl revealed that the main cairn had a complex structural development with two cists, one of which had a whetstone and cremated bone deliberately hidden within the structure. A smaller, nearby, cairn had been robbed but still retained an intact cremation deposit. It is argues that the main cairn was situated on a false-crest, inter-visible with putative Bronze Age settlement in the valley below. Appendices include reports on the cremations, phosphate and heavy mineral analyses of soil deposits and a catalogue of all the then-known mountain-top cairns in Snowdonia.

In archaeological research designs that focus on sites in coastal and shorebound areas, a short geographical distance is often equated with a high degree of functional correlation between settlement and water without any further investigations of this (pre-)supposed relationship. This is both a theoretical and a methodological problem: instead of testing a hypothesis against the empirical material as the result of actions carried out by prehistoric people, a vaguely characterized empirical pattern is argued to reflect the inherent interrelationship to water. This article presents a process of generating and applying appropriate methodological approaches in the study of water-bound strategies. It explores a site with an initially unknown character and date, but with the remains of a still monumental artificial earthen wall standing close to what was hypothesized to be a former shore zone at Garn, in east central Sweden, and delves into how water-bound strategies might be expressed and investigated in archaeology.

Boplatsvallar, often translated as semi-subterranean settlements, is an ancient monument with a diffuse definition. Defined as -embankments that partially or completely surround a often lowered/dug down surface- this category of ancient monuments is also made up of a former category which traditionally was interpreted as winter settlements from the late Stone age in Sweden. This view of the ancient monuments carried over, to a certain extent, to this new definition. Should this be the case, that this category of monuments are remains of winter settlements, used recurringly over an extended period of time, then they should exhibit similar signasl in regards to the distribution of the anthropogenically altered soil chemical and soil physical properties ath the sites.
The area around Lillsjön, Anundsjö parish, Ångermanland, have four "boplatsvallar" located separately in the regional area. This means they can be considered single contexts suitable to test the aforementioned hypothesis.
The result of the intra-site study indicates that the sites have been used differently. Two of the sites exhibit a more local distribution of the heightened values of phosphates and magnetic susceptibility, distributed close around the ancient monument itself. The other two sites have a distribution of heightened values distributed over a larger area around the monuments, where one of them shows no particular difference from the background values at the site. This result thus suggests that there is a difference in how these "boplatsvallar" have been used prehistorically.

"The cooperation of archaeologists with representatives of other scientific disciplines has a long tradition. In Central Europe there has been an especially strong relationship between archaeology and history. With the emergence of culture-historical archaeology, with its special focus on ethnicity and ethongenesis, to find arguments in support of its principles researchers turned to methods such as settlement geography. This opened up the way to an increasingly intimate relationship with nature sciences. In Upper Silesia a closer cooperation of archaeologists with representatives of other disciplines dates from the first half of the twentieth century, with a heyday from the 1970s onwards. Cooperation, at first in the form of non-regular expert studies, with time generated a basis for multi-faceted interdisciplinary research projects. Nowadays projects of this sort continue to grow in number and cover diverse types of archaeological site – from the campsites of Palaeolithic hunter-gatherers to urban sites, castles and palaces of the early modern age.
Cooperation with specialists in nature sciences is particularly intensive. Accurate recording of archaeological finds during excavation makes it necessary to join forces with specialists in geodesy and cartography, and also, to use remote detection methods and photogrammetry. In non-destructive investigation of the archaeological record a special role is played by cooperation with geophysicists. Stratigraphy, the basic method for determining the relative age of archaeological finds, was borrowed from geology. Progressive methods of absolute dating used for determining the true age of artefacts are the province of specialist laboratories. Precise dating of timber features is possible thanks to cooperation with dendrologists and dendrochronologists. Thanks to physicists archaeologists can obtain absolute age determinations making use of physical phenomena such as radioactive isotope decay (radiocarbon, potassium-argon and uranium-thorium dating).
A vital aspect of archaeological research is the interaction of humans with their natural environment. These are studied in three ways: through analysis and assessment of the ancient environment, one contemporary with the archaeological features, palaeoenvironmental studies which make it possible to reconstruct the environment, and specialist analyses of assorted environmental data recovered during fieldwork (animal bones, plant macro-remains, plant pollen, insects, lithic resources, etc.). These studies call for a close cooperation with many specialists: geographers, geologists, geomorphologists, pedologists, hydrologists, petrographers, demographers, pollen specialists, botanists, zoologists, ceramographers, metallographers, etc.
A vast body of potential data on the life of ancient communities is to be found in the skeletal remains recovered from cemeteries and in the forms of burial when these are submitted for analysis to osteologists.
Other crucial studies focus on production and technology and can be pursued thanks to cooperation with nature scientists and specialists in technical sciences. Different artefact categories are subjected to specialist analyses to determine their material, area of origin and to reconstruct processes used in manufacturing individual categories of objects and the level of sophistication of technology. Next to archaeological objects archaeologists discover built structures – the remains of dwellings, storage pits, sacred sites, etc. Their study requires cooperation with ethnographers, historians of architecture, civil engineering and art.
Increasingly more often archaeologists are turning their attention closer to the modern period. Archaeology of the more recent past unavoidably comes into contact with diverse categories of written and iconographic evidence and cannot function without cooperation with historians, representatives of auxiliary sciences of history and art historians. An important role is played by numismatics. Coins are useful for dating archaeological assemblages. Linked inextricably with trade and exchange they had also other uses and a symbolic meaning as well, one associated with their issuer, his environment, place of deposition, etc.
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The recommended analysis of phosphate which is by now approved in practice, demonstrates an economic form of Bleck’s method of analysis. Thanks to method suitability for routine analysis more than 100 samples a day can easily be measured and evaluated. As the procedure of analysis comes along with a reduction of reagent quantities, not only the consumption of vanadate, molybdate and nitric acid is reduced. Only a minimal part of the generally used reagents quantity reaches the waste disposal, also. In this way, for example, our consumption of vanadate to 0.5mg per soil sample is calculated.

""Im Bereich von »Lungenkärchen« bei Mendig wurde eine neue Axialhofanlage entdeckt. Sie weist ein Hauptgebäude im Reihentyp, ein großes Wasserbecken sowie sieben Nebengebäude teils bekannter Funktion auf. Die Fundstelle wird exemplarisch für eine Reihe von mehreren reichen villae rusticae im unmittelbaren Umfeld der Mühlsteinbrüche untersucht, die dort in exzeptionell hoher Dichte vorliegen. Auf die zum großen Teil außerhalb der Landwirtschaft verankerte ökonomische Grundlage könnten die vergleichsweise kleine pars rustica und die nur durchschnittlich bemessene Wirtschaftsfläche der villa von »Lungenkärchen« weisen. Der enge räumliche Bezug zu den Steinbrüchen, die
Mühlsteinrohlinge im Villengelände sowie Parallelen wohlhabender römischer Landsitze nahe anderen Steinbrüchen belegen in hohem Maße einen Profit von dem Export der Steine. Hier sowie in den umliegenden Großvillen residierten demnach die Besitzer der Mühlsteinbrüche. Im Gegensatz zu dem vicus von Mayen erfolgte im nördlichen Umfeld des römischen Industriereviers ab etwa 100 n. Chr. bis mindestens in das 3. Jahrhundert eine monumentalisierende Landnutzung, die dem gesteigerten Repräsentationsbedürfnis der hiesigen Elite entsprach.

De riches propriétaires de carrières? La villa à »pavillons multiples alignés« de »Lungenkärchen« près de Mendig (Lkr. Mayen-Koblenz) dans le contexte de l’occupation du sol à l’époque romaine
Une nouvelle villa à »pavillons multiples alignés« a été découverte sur le territoire de »Lungenkärchen« près de Mendig. Elle présente un bâtiment principal à pièces en enfilade, un grand bassin et sept bâtiments annexes dont la fonction est établie pour certains. Ce site fait l’objet d’une étude à titre d’exemple pour une série de riches villae rusticae situées à proximité immédiate des meulières dont la concentration est très élevée dans cette région. La pars rustica relativement modeste et les dimensions moyennes de la surface utilitaire de la villa de »Lungenkärchen« signalent peut-être des ressources économiques essentiellement extérieures à l’agriculture. La proximité des carrières, les ébauches de meules sur le terrain de la villa ainsi que des domaines aisés comparables dans le voisinage d’autres carrières témoignent clairement du profit tiré de l’exportation des pierres. Ainsi, c’est ici comme dans les autres grandes villas que devaient habiter les propriétaires des meulières. au nord du bassin industriel romain, contrairement au vicus de Mayen, se développe à partir d’environ 100 ap. J.-C. jusqu’au 3e siècle au moins une exploitation du sol monumentale, correspondant au besoin accru de représentation des élites locales. Traduction: Y. Gautier""

This paper summarizes the results of geoarchaeological studies undertaken in the last few years at Palaeolithic and Neolithic sites in south-western Poland. In the following paragraphs applied methods are reviewed. Very valuable were microstratigraphic investigation which shed light on site formation processes of the Upper Palaeolithic sites as well as provide a set of data on microfossils contained in palaeosoils and the settlement floor. The isotopic studies of Pleistocene faunal remains yielded important data on palaeotemperatures at the time of human occupation connected with the late stage of the Middle Palaeolithic. Finally the geophysical prospection. with the use of magnetometer, combined with geochemical analysis of phosphate content in soil enabled to characterize and identify functional variability of Neolithic settlements