Pigment analysis by Raman microscopy and portable X-ray fluorescence (pXRF) of thirteenth to fourteenth century illuminations and cuttings from Bologna

Non-destructive pigment analysis by Raman microscopy (RM) and portable X-ray fluorescence (pXRF) has been carried out on some Bolognese illuminations and cuttings chosen to represent the beginnings, evolution and height of Bolognese illuminated manuscript production. Dating to the thirteenth and fourteenth centuries and held in a private collection, the study provides evidence for the pigments generally used in this period. The results, which are compared with those obtained for other north Italian artwork, show the developments in usage of artistic materials and technique. Also addressed in this study is an examination of the respective roles of RM and pXRF analysis in this area of technical art history

Geo-material provenance and technological properties investigation in Copper Age menhirs production at Allai (central-western Sardinia, Italy)

During the 2nd millennium BC anthropomorphic menhirs belonging to a 3rd millennium BC sanctuary were reused as building material in the Arasseda Nuraghe (Sardinia, Italy). To analyse the Arasseda menhirs and the local Monte Ironi geological samples (presenting similar visual features), chemical (pXRF, ICP-OES, ICP-MS), mineralogical-chemical (PXRD) and physical (Mohs hardness) measurements were performed. Through the experimental data, the menhirs source provenance and the technological properties (workability, durability) of the raw material chosen for sculptural purposes during Copper Age were investigated. To the authors’ knowledge this is the first archaeometric study on the Arasseda menhirs (the third on Sardinian menhirs) and one between the few recently developed on European megaliths

Quick Analysis of Organic Amendments via Portable X-ray Fluorescence Spectrometry

The determination of heavy metals in soils and organic amendments, such as compost, manure, biofertilizer, and sludge, generally involves the digestion of samples with aqua regia, and the determination of those in the solution using various techniques. Portable X-ray fluorescence (PXRF) has many advantages in relation to traditional analytical techniques. However, PXRF determines the total elemental content and, until now, its use for the analysis of organic amendments has been limited. The objective of this work is the calibration of a PXRF instrument to determine the aqua regia-soluble elemental contents directly in solid samples of organic amendments. Our proposal will avoid the digestion step and the use of other laboratory techniques. Using a training set of samples, calibration functions were obtained that allow the determination of the aqua regia-soluble contents from the PXRF readings of total contents. The calibration functions (obtained by multiple linear regression) allowed the quantitative determination of the aqua regia-soluble contents of Fe, K, P, S, Zn, Cu, Pb, Sr, Cr, and Mn, as well as the organic matter content and a semi-quantitative assessment of Al, Ca, V, Ba, Ni, and As contents. The readings of Si, Fe, Al, Ca, K, or S were used as correction factors, indicating that the calibrations functions found are truly based on the chemical composition of the sample matrix. This study will allow a fast, cheap, and reliable field analysis of organic amendments and of other biomass-based materials.Spanish Ministry of Science, Innovation and Universities, and the European Regional Development Fund, European Union, (AEI/FEDER, UE), grant number CGL2016-78937-R

Shuttle rocket booster computational fluid dynamics

Additional results and a revised and improved computer program listing from the shuttle rocket booster computational fluid dynamics formulations are presented. Numerical calculations for the flame zone of solid propellants are carried out using the Galerkin finite elements, with perturbations expanded to the zeroth, first, and second orders. The results indicate that amplification of oscillatory motions does indeed prevail in high frequency regions. For the second order system, the trend is similar to the first order system for low frequencies, but instabilities may appear at frequencies lower than those of the first order system. The most significant effect of the second order system is that the admittance is extremely oscillatory between moderately high frequency ranges

A (not so) dangerous method: pXRF vs. EPMA-WDS analyses of copper-based artefacts

Analysis of metal objects with portable and handheld X-ray fluorescence spectrometry has become increasingly popular in recent years. Here, methodological concerns that apply to non-destructive, surface examination with XRF instruments of ancient metal artefacts are discussed based on the comparative analyses of a set of copper-based objects by means of portable X-ray fluorescence (pXRF) and electron probe microanalyser (EPMA). The analytical investigation aims to explore issues of instrument comparability and reliability of the non-invasive pXRF results. The different analytical approaches produce a comparable pattern for the major element concentrations, but substantial variation is evident when it comes to the absolute values for major and minor/trace elements

Ceramic composition at Chalcolithic Shiqmim, northern Negev desert, Israel: investigating technology and provenance using thin section petrography, instrumental geochemistry and calcareous nannofossils

Technological innovations in ceramic production and other crafts are hallmarks of the Chalcolithic period (4500–3600 BCE) in the southern Levant, but details of manufacturing traditions have not been fully investigated using the range of analytical methods currently available. This paper presents results of a compositional study of 51 sherds of ceramic churns and other pottery types from the Chalcolithic site of Shiqmim in the northern Negev desert. By applying complementary thin section petrography, instrumental geochemistry and calcareous nannofossil analyses, connections between the raw materials, clay paste recipes and vessel forms of the selected ceramic samples are explored and documented. The study indicates that steps in ceramic manufacturing can be related to both technological choices and local geology. Detailed reporting of the resulting data facilitates future comparative ceramic compositional research that is needed as a basis for testable regional syntheses and to better resolve networks of trade/exchange and social group movement

Using handheld pXRF to study medieval stained glass: A methodology using trace elements

The surfaces of 30 pieces of glass from panel 3b of the Great East Window of York Minster (1405-1408 CE) were analyzed by handheld portable X-ray fluorescence (pXRF) and small samples from the same pieces were analyzed by electron microprobe (EPMA). Comparison of the two methods reveals significant divergences which are not systematic, particularly for elements lighter than Ti. Rather than a problem with pXRF calibration or correction software, the non-systematic error is attributable to the presence of a thin surface layer of weathered glass. Analysis of the depths of X-ray generation indicate that virtually all X-rays characteristic of Ca and K are generated within the top 50 µm of the glass. However, for heavier elements such as Rb, Sr and Zr, most emitted X-rays are generated below 100 µm. Using pXRF data for the heavier elements, it is possible to replicate the compositional groupings identified by quantitative EPMA. White glass in the window is likely to have originated in England, while colored glasses were probably obtained from the Continent. The alkali contents of the green and yellow glasses appear to have been manipulated to generate their colors. Glass which is medieval in technology but not original to the panel was identified. In particular, zirconium proved a useful indicator of glassmaking regions, and rubidium and strontium were more sensitive to differences between batches, which has interesting implications for future work

Ancient technology and punctuated change: Detecting the emergence of the Edomite Kingdom in the Southern Levant.

While the punctuated equilibrium model has been employed in paleontological and archaeological research, it has rarely been applied for technological and social evolution in the Holocene. Using metallurgical technologies from the Wadi Arabah (Jordan/Israel) as a case study, we demonstrate a gradual technological development (13th-10th c. BCE) followed by a human agency-triggered punctuated "leap" (late-10th c. BCE) simultaneously across the entire region (an area of ~2000 km2). Here, we present an unparalleled, diachronic archaeometallurgical dataset focusing on elemental analysis of dozens of well-dated slag samples. Based on the results, we suggest punctuated equilibrium provides an innovative theoretical model for exploring ancient technological changes in relation to larger sociopolitical conditions-in the case at hand the emergence of biblical Edom-, exemplifying its potential for more general cross-cultural applications

Mobile spectroscopic instrumentation in archaeometry research

Mobile instrumentation is of growing importance to archaeometry research. Equipment is utilized in the field or at museums, thus avoiding transportation or risk of damage to valuable artifacts. Many spectroscopic techniques are nondestructive and micro-destructive in nature, which preserves the cultural heritage objects themselves. This review includes over 160 references pertaining to the use of mobile spectroscopy for archaeometry. Following a discussion of terminology related to mobile instrumental methods, results of a literature survey on their applications for cultural heritage objects is presented. Sections devoted to specific techniques are then provided: Raman spectroscopy, X-ray fluorescence spectrometry, Fourier transform infrared spectroscopy, laser-induced breakdown spectroscopy, and less frequently used techniques. The review closes with a discussion of combined instrumental approaches

O Tumulus 1 do Souto (Abrantes, Médio Tejo): Novos contributos para o conhecimento das materialidades do mundo funerário do Bronze Final no Centro de Portugal

O artigo apresenta e discute os resultados obtidos das análises arqueométricas realizadas sobre 4 fragmentos de metal, 1 fragmento de cerâmica de uma grande urna e sobre as marcas/incrustações encontradas na superfície de um pequeno púcaro procedentes de um contexto funerário de incineração atribuído ao Bronze Final (BF), o Tumulus 1 do Souto (Abrantes, Centro de Portugal). O sítio arqueológico e os materiais recuperados já foram publicados por um dos autores, mas o estudo arqueométrico dos materiais, em particular dos fragmentos de metais e das cerâmicas nunca foi efetuado. De acordo com uma abordagem multi-analítica recorreu-se a diversas técnicas analíticas, nomeadamente Espectrometria de Raios-X Portátil (pXRF), Microscopia Eletrónica de Varrimento acoplada a Detector de Raios-X por Dispersão de Energias (SEM-EDS), Microscopia óptica (MO) e Difração de Raios-X (XRD). Os resultados obtidos determinaram a proveniência da grande urna, provavelmente produzida com materiais encontrados num raio de 10-15 km do sítio arqueológico. A composição química e as características dos fragmentos de metal analisados indicam tratar-se de uma liga binária (Cu+Sn) com pequenas inclusões de elementos secundários como prata, arsénio e ferro. O estudo também evidenciou, na superfície do pequeno púcaro, a presença de uma patina metálica. A combinação dos dados arqueológicos e arqueométricos permitiu aumentar o conhecimento do estado da arte no contexto funerário de cremação com deposição em urna, típico da Idade do Bronze no Oeste da Península Ibérica, especialmente no médio Tejo