Isolation and Isotopic Analysis of Individual Amino Acids from Archaeological Bone Collagen: A New Method Using Rp‐hplc

This paper presents a new method for the isolation and isotopic analysis of some individual amino acids from proteins. The technique and its constituent steps are discussed; then isotopic analyses of amino acids from several samples of bone collagen from the Late Roman site of Poundbury, Dorset, UK are presented. The applications of the method are discussed, as well as some advantages of this technique relative to other methods. Although developed for use with archaeological bone collagen, the technique is equally applicable to other proteinaceous materials. The use of reversed‐phase HPLC avoids problems of isotopic fractionation inherent in using ion‐exchange HPLC. Amino acids are isolated preparatively, allowing both carbon and nitrogen isotopic values to be measured on a single sample using CF‐IRMS. Since amino acids are isotopically analysed in an underivatized form (unlike GC‐C‐IRMS), the method also presents the possibility of collecting the CO₂ generated during CF‐IRMS: this would allow the subsequent dating by ¹⁴C‐AMS of individual amino acids isolated from archaeological samples.     

Evidence for Varying Patterns of Exploitation of Animal Products in Different Prehistoric Pottery Traditions Based on Lipids Preserved in Surface and Absorbed Residues

The excavation of a barrow at Upper Ninepence, Walton in the Welsh Borderlands, U.K., revealed two phases of occupation associated with two different ceramic traditions, namely Grooved Ware (2500bc) and Peterborough Ware (3000bc). The Grooved Ware and Peterborough Ware pits seem to have a mutually exclusive distribution on the site. Screening of the sherds for lipid residues has revealed the presence of remnant fats in a remarkably well-preserved state considering the age of the finds. Investigations of various chemical characteristics of the remnant fats from absorbed and carbonized residues have enabled distinctions to be drawn between fats from non-ruminant (e.g. porcine) and ruminant (e.g. ovine or bovine) origins. Significantly, both ruminant and non-ruminant fats are found associated with the Grooved Ware whereas only ruminant fats are found associated with the Peterborough Ware. The assignments are based upon the distributions of solvent-extractable lipid components and the compound-specific stable carbon isotope values of the major n -alkanoic acids. The results reveal differences in vessel use and indicate possible changes in patterns of animal exploitation or dietary preferences between the two phases of occupation. The results illustrate the importance of residue analysis in archaeological investigations, particularly at prehistoric sites where evidence from faunal remains is limited or absent.     

PALAEOCLIMATIC IDENTIFICATION BASED ON AN ISOTOPE STUDY OF TRAVERTINE FROM THE COPPER AGE SITE AT LOS MILLARES,SOUTH-EASTERN SPAIN*

Remains of an aqueduct from the Copper Age settlement of Los Millares have been studied. The isotope results (—7‰ < δ¹⁸O — 5.3‰) show that the aqueduct was used to transport fresh water at room temperature. The results are inconsistent with the aqueduct being used for hot water transport or as a container for water exposed to evaporation processes. Both isotopic and mineralogical results were useful in identifying the origin and use of building materials and also in determining climatic conditions during the time of the settlement occupation.     

PETROGRAPHIC AND ISOTOPIC CHARACTERIZATION OF THE MARBLE OF THE ISLAND OF TINOS (GREECE)*

Most outcrops of good‐quality crystalline marble in Mediterranean countries were exploited in Greek and Roman times. Hence, a wide variety of marble is now found in archaeological excavations. The precise determination of the provenance of a marble object is of great archaeological importance, and is now mostly obtained by coupling the petrographic study of a thin section with the analysis of the C and O stable isotopes, or by stereomicroscopy and EPR. The existing databases are considerable but still insufficient, because our knowledge about and study of ancient Mediterranean quarries remain incomplete. The contribution of this research is to add new petrographic and isotopic data on small quarries on the Greek island of Tinos that were exploited in antiquity. This marble belongs to the same geological horizon; it is quite pure, sometimes dolomitic and characterized by a low‐T, high‐P metamorphism that produced a limited recrystallization (MGS varying from 0.64 to 2.50 mm) on marine limestone protoliths. The petrographic features are quite distinctive: the fabric is strongly lineated and often stressed; and the accessory minerals are ubiquitary quartz, ore minerals, graphite and muscovite. As far as the isotopic data are concerned, δ¹³C_PDB varies from 1.1 to 2.7, and δ¹⁸O_PDB from ?1.7 to ?11.4. Both the features and the data have been compared with those of similar marbles used in antiquity, showing that their combination mirrors the fingerprint of the Tinos marble.     

Infrared and Isotopic Evidence for Diagenesis of Bone Apatite at Dos Pilas, Guatemala: Palaeodietary Implications

The use of stable carbon isotopic analysis of bone apatite to reconstruct prehistoric diets is hindered by the possibility of diagenetic alteration of carbonate during burial. We examine apatite preservation in Classic Period Maya skeletal remains from Dos Pilas, Guatemala, using Fourier transform infrared spectroscopy (FTIR). We use weight % CO₂evolved from apatite, FTIR carbonate/phosphate absorbance ratios, phosphate peak splitting crystallinity indices, fluoride peaks, and stable oxygen isotopic ratios to identify diagenetic change in apatite chemistry. Isotopically light carbon taken up from burial soil is adequately removed from most Dos Pilas bone by treatment with dilute acetic acid, but more severe alteration cannot be reversed by standard preparation methods. Infrared criteria identify recrystallized apatite in a subset of Dos Pilas burials, that is accompanied by isotopic exchange, and that no longer preserves biogenic δ¹³C. These results illustrate that comparatively recent bone may be diagenetically altered and demonstrate a need for systematic evaluation of mineral integrity in all archaeological bone prior to interpreting paleodiets with apatite δ¹³C.     

PROVENANCE STUDY OF MARBLE ARTEFACTS FROM THE ROMAN BURIAL AREA OF FASCHENDORF (CARINTHIA,AUSTRIA)*

Numerous marble artefacts were among the extraordinary findings excavated at the Roman burial area of Faschendorf (Carinthia, Austria). The provenance of marble objects, particularly in the Roman provinces, is mostly unclear. Predominantly Mediterranean marbles have been used, but there are also some marble occurrences in the eastern Alpine regions that were exploited in those times. Besides a mineralogical–petrographic analysis, grain‐size evaluation in particular, and the determination of carbon and oxygen isotopes allow an effective characterization of the Faschendorf materials. Their provenance from the Gummern Marble complex in Carinthia is very likely.     

SCIENTIFIC CHARACTERIZATION OF THE POHORJE MARBLES,SLOVENIA

As a former part of the great Roman Empire, Slovenia has many archaeological sites featuring buildings and objects entirely or partly constructed from marble whose provenance is doubtful. In Slovenia, the most probable source of such marble is the Pohorje Mountains. For the purpose of supporting further provenance studies, these marbles are fully scientifically characterized. The techniques used are petrographic and geochemical analysis, stable isotope ratio analysis and EPR spectroscopy. The results show that the Pohorje marbles are highly heterogeneous in both their isotopic and geochemical parameters as well as grain sizes. The parameters of the different Pohorje marble outcrops are compared between themselves and with the parameters of known ancient quarries in the Mediterranean and Austria. The use of a multi‐technique approach with combined parameters allows the best possible discrimination.     

ON ISOTOPES AND OLD BONES*

This review charts the developments and progress made in the application of stable light isotope tools to palaeodietary adaptations from the 1970s onwards. It begins with an outline of the main principles governing the distribution of stable light isotopes in foodwebs and the quality control issues specific to the calcified tissues used in these analyses, and then proceeds to describe the historical landmark studies that have marked major progress, either in their archaeological applications or in enhancing our understanding of the tools. They include the adoption of maize agriculture, marine‐focused diets amongst coastal hunter–gatherers, trophic level amongst Glacial‐period modern humans and Neanderthals, and the use of savannah resources by early hominins in Africa. Particular attention is given to the progress made in addressing the challenges that have arisen out of these studies, including issues related to the routing of dietary nutrients. I conclude with some firm, and some more speculative, pointers about where the field may be heading in the next decade or so.     

A NEW METHOD FOR THE DETERMINATION OF THE PROVENANCE OF WHITE MARBLES BY CHEMICAL ANALYSIS OF INCLUSION FLUIDS: THE MARBLES OF THE MAUSOLEUM OF BELEVI/TURKEY*

A new method is presented in this paper to pinpoint the origin of white marbles using the chemical analysis of fluids occurring as micro-inclusions in calcitic or dolomitic marbles. Beside the conventional methods usually applied for this purpose, the analyses of significant anions and cations in fluids extracted from white marbles were used to characterize different types of marbles. Using this new approach it is possible to distinguish different groups of marbles which cannot be separated isotopically. A case study was performed on the mausoleum of Belevi, close to Ephesus in Turkey, and the quarries in the area of the mausoleum. The marbles used for the architecture of the mausoleum cannot be distinguished isotopically but were split into two groups when using fluid inclusion analysis. The corresponding quarry for the high-quality marble (cella walls, columns etc.) turned out to be the Kentli Çiftliği quarry, which also supplied the marbles for the classical Artemision. According to the chemical and fluid data it can be shown, however, that neither the adjacent famous antique quarry of Belevi nor the underground mine of Kusini, some 5 km away from the mausoleum, are the sources for the marbles used for the construction or decoration of the mausoleum.     

DETECTION OF ANCIENT MARBLE FORGERY: TECHNIQUES AND LIMITATIONS*

Since 1960, scientific results have replaced aesthetic judgements in marble authentication studies and the technology to perform analytical tests on micro‐samples has developed rapidly. However, no single method can be used to determine the authenticity of a piece of marble. A ‘detective‐like’ investigation is usually adopted by using optical microscopy, ultraviolet‐induced fluorescence, provenance determination techniques and mineralogical, chemical and morphological analyses of the patina. A newly proposed thermoluminescence methodology calculates the ‘burial age’ of recently excavated objects or distinguishes artefacts exposed to sunlight since antiquity from those exposed recently. The technique shows a lot of potential; however, much work remains to be done.     

How Did Mississippians Prepare Maize? The Application of Compound‐Specific Carbon Isotope Analysis to Absorbed Pottery Residues From Several Mississippi Valley Sites

A newly developed compound‐specific stable carbon isotope technique allows the detection of maize in absorbed organic pottery residues. This method was applied to absorbed organic residues from a variety of Mississippi Valley potsherds, and successfully identified maize components. Maize was cooked in sampled vessels less often than expected, but otherwise fitted expected patterns of maize use derived from stable carbon isotope analysis of human bone from the region. Absorbed organic pottery residue analysis is useful in determining pottery use, particularly in concert with other analytical methods.     

PETROGRAPHIC AND STABLE ISOTOPE ANALYSES OF LATE CLASSIC ULÚA MARBLE VASES AND POTENTIAL SOURCES*

Ulúa marble vases from the Ulúa Valley of northwestern Honduras are a hallmark luxury good from Late Classic (ad 600–900) Mesoamerica. Archaeological and stylistic data point to centralized production at one site, Travesía. This paper analyses stable isotope and petrographic data from the vases and three potential procurement areas. The results indicate that the vases were produced from one primary source with one, potentially two, secondary sources. Procurement patterns most probably corresponded to contemporary communication routes. The results clearly indicate that a multi‐method approach is necessary for sourcing marble from Honduras.     

MINERO‐PETROGRAPHIC AND GEOCHEMICAL CHARACTERIZATION OF ‘GRECO SCRITTO’ MARBLE FROM CAP DE GARDE,NEAR HIPPO REGIUS (ANNABA,ALGERIA)*

This work presents the results of the first mineralogical, petrographical and geochemical characterization of the marble quarried from the Cap de Garde headland, not far from Annaba (Algeria). This site is traditionally held by archaeologists to be the main source of supply of the so‐called ‘greco scritto’ marble, which was much used by the Romans for architectural and decorative–ornamental purposes, locally from the first century bc , and in Rome and central and southern Italy from the late Flavian period until the fourth century ad . The databank relating to the quarried material, created here for the first time, is used to establish the origin of ‘greco scritto’ found in six important Roman cities of North Africa: Hippo Regius and Cuicul (Djemila), in Algeria; Volubilis, in Morocco; Cyrene, in Libya; and Carthage and Utica in Tunisia. The results of this archaeometric study support the hypothesis (already put forward by authors) that the ‘greco scritto’used in the Roman Mediterranean originated from different sites, and suggest the existence of a number of North African quarries, also in the vicinity of Annaba.