SEM/EDS

This article reports the results of an investigation into the efficiency of mechanical activation to increase the reactivity in alkali activated mortar synthesized from low-grade clay. Mechanical activation significantly changed the structure of clay, increasing the specific surface area, and decreasing the particle size. The 7-day compressive strength of mortar synthesized from untreated clay was 31.7 MPa, which increased to 35.3 after 4 h milling. A further increase of grinding time to 8 h did not result in any increase in compressive strength which is attributed to a decrease in the workability. However, the extent of reactivity did significantly increase as determined from solid-state MAS NMR, FTIR, and EDS analyses. Solid-state MAS NMR results revealed the increased formation of Q 4 (2Al) silicon sites, which is correlated with improved reaction. Furthermore, the EDS and FTIR analysis results indicated greater incorporation of aluminium into the matrix structure with increased grinding time.

Since the Early Neolithic, salt has played an important role in the social and economic development of populations. Consequently, the study and comprehension of salt management strategies have become a significant component of current archaeological research. This study is part of an interdisciplinary research program consisting of excavations and detailed analyses on two Early Neolithic salt working sites situated in the sub-Carpathian region of Romania, Lunca and Tolici (county Neamt¸ ). These
remarkably well-preserved sites are characterised by stratified deposits several meters thick. Detailed stratigraphic descriptions were followed by optical microscopy analysis (soil micromorphology) and scanning electron microscopy (SEM) coupled with geochemical analysis (EDS). The aim of these analyses was to identify specific sedimentary, petrographic and chemical characteristics that could be linked to salt working process. The results enable us to describe the main site formation process over time and to detect chemical components of edible salt (Na and Cl) in Early Neolithic ashes. These new data consolidate previous interpretations of the operating procedures implemented from the Early Neolithic to the Bronze Age. Two techniques appear to have been preferentially adopted: pouring natural brine onto combustion structures during the Early Neolithic and evaporation in specific ceramic containers from the Chalcolithic onwards.

Epiphytic lichens are efficient air pollution bio monitors as they obtain nutrients, water and pollutants from the atmosphere. The aim of this study was at analyzing the surface of hyphae and the surface of the lichens Evernia prunastri (unwashed and washed in distilled water). Mass percentage of 26 selected elements: C, O, Na, Mg, Al, Si, P, S, Cl, K, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Cd, Sn, Sb, Hg, Pb and Bi was determined by scanning electron microscopy (SEM) and energy‐dispersive X‐ray spectroscopy (EDS). Mass percentage of: Na, Mg, V, Cr, Mn, Co, Ni, Zn, As, Cd, Sn, Sb, Hg, Pb was below the limit of detection of the applied method. The mass percentage of all other determined elements on the hyphae and surface of lichen was higher in unwashed samples, except for C, O, P, Fe, Cl, Ca and Cu. The elemental analysis of the unwashed lichen surface showed the prevalence of: O, C, Si, Cu and
Bi. Results obtained in the unwashed and washed lichen samples showed that the cleaning with water can be used in order to eliminate adhering materials. Indeed, most of elements of interest for the environmental contamination accumulated by the lichens were not
removed. SEM images showed particles that are flat, with irregular shape and edges, generally smooth and rounded indicating that the particles deposited were dry aerosol particles.

Global food shortage is mainly due to the post-harvest spoilage of food, rather than its under-production, especially in the sub-Saharan African countries. Rapid detection tools for the spoilage of fruit such as banana (Musa acuminata) would be a great resource in alleviating losses during post-harvest storage. In this study, silver-based colloidal nanoparticle (AgNPs) solution was synthesized using culture supernatant or wet biomass (cell pellets) of Bacillus subtilis. The synthesized silver nanoparticles solution was confirmed using UV-Vis Spectrophotometer and further characterized using Scanning Electron Microscope (SEM), X-ray Diffractometer (XRD) and Fourier Transmission Infrared (FT-IR), and then evaluated as a colorimetric sensor for the volatile compound released during the deterioration of Musa acuminata. The original reddish brown colour of the silver nanoparticle solution changed to light brown by the end of the fourth day and finally turned transparent on the tenth day. Simultaneous analysis carried out by UV-Vis spectroscopy corroborates our investigation of AgNPs as a colorimetric sensor displaying selectivity and specificity for 1,2-Benzenedicarboxylic acid, bis (2-methyl propyl) ester which was released during the deterioration of Musa acuminata. The use of colorimetric sensor as conducted in this study will help in easy detection for control of crop deterioration.

however, subtle processes which involve the specimen, the however, subtle processes which involve the specimen, the electron beam and any mobile species on the sample electron beam and any mobile species on the sample surface frequently cause the build up of hydrocarbon surface frequently cause the build up of hydrocarbon contamination layers. contamination layers.

Gunshot residue (GSR) analysis by scanning electron microscopy/energy dispersive x-ray spectrometry (SEM/EDX) is routinely performed in forensic science laboratories. At the end of 2011, a field emission gun (FEG)-SEM was installed at the authors' laboratory for this type of examination. Following the installation of the FEG-SEM, an extensive process was conducted, in order to determine the optimal operating parameters of this instrument for GSR analysis. Because the nature of synthetic GSR samples (such as the European Network of Forensic Science Institutes GSR2011 proficiency test sample) is significantly different from casework samples, it was decided not to use them for this purpose. Instead, a GSR casework sample, previously analyzed by tungsten-filament SEM as part of the laboratory's routine examinations, was selected. This sample was repeatedly analyzed (more than 200 times), under different operating conditions. The main parameters that were examined for the FEG-SEM were the electron source accelerating voltage, the backscattered electrons image acquisition time, the magnification, the backscattered electrons image resolution, and the energy-dispersive X-ray spectrometry acquisition time. The smallest detected feature was calculated by the software, based on the set image resolution and magnification. For each set of parameters, the detected GSR particles were recorded, in addition to the total number of detected particles and the time taken for the run. It was found that for a given smallest detected feature, the effective search conditions were higher magnification and lower number of pixels per line. The present work includes a detailed description of the optimization process and its results. The process utilized in this work is applicable for other laboratories conducting similar type of GSR analysis as well.

MacDonald, B.L. The Analysis of Inorganic Pigments using Spectrometric Techniques. In, The Unvarnished Truth: Exploring the Material History of Paintings. Edited by B.L. MacDonald, N. Hathaway, C. Podedworny. McMaster Museum of Art: Hamilton, Canada. Distributed by Art Books Canada, Montreal. pp. 53-61.

Non-metallic inclusions are a major issue during the production clean steels, as they influence the microstructure and structural properties effectively. They are often considered as harmful to the final product quality and to the steel processing productivity; therefore many industrial efforts are directed towards improving inclusion removal. Another way is to use non-metallic inclusions to produce steels with enhanced properties. In both cases, the key issue is to control the characteristics of the inclusion population in the liquid steel, such as quantity/limit, composition, physical appearance or morphology, shape, size and distribution. The application of new secondary refining techniques and non-metallic inclusion reduction techniques in steel production processes has greatly reduced the size and amount of nonmetallic inclusions remaining in molten steels and steel products due to which inspection of inclusions is very difficult. The influences of inclusions on the properties of steels are discussed. As inclusions have influence on several properties of steel, such as formability, toughness, and machinability and corrosion resistance. In general, the less severe the inclusions, the higher quality of steel. This is the reason for, analysing and assessment of non-metallic inclusions is important for quality control. The main part of this work has been a literature survey, reviewing the main methods used for the characterization of inclusions in clean steels, experimental reports for information on how steel cleanness is evaluated today, and how the steel cleanness is related to the performance of clean steels as a product.

H13 tool steel with excellent hot working properties is commonly used for manufacturing dies. However, the damage of die surface due to cyclic thermo-mechanical loading is detrimental to the service life. In order to enhance the die life, it has been observed that cladding based repair is superior to welding or thermal spraying repair techniques. In this paper, experimental study of laser cladding of H13 has been carried out. CPM 9V steel powder has been deposited on H13 tool steel plate for repairing the die surface damage using a CW CO 2 laser in conjunction with powder injection system. The effect of laser parameters on clad geometry and clad quality has been investigated. The microstructure of laser cladded samples has been characterized using optical microscope (OM) and scanning electron microscope (SEM). The phases and the residual stresses present in the clad have been determined via X-ray diffraction. The micro-hardness profiles obtained in the clad–substrate system and the hardness change due to cyclic thermal loading have also been characterized. Optical micrographs of the clad microstructure shows existence of vanadium carbide particles embedded in martensite and retained austenite. The hard vanadium carbide particles increase the clad hardness to an average of four times greater than the substrate hardness. It has been observed that compressive residual stresses are generated in clad which is desirable for repair applications as it will impede the crack propagation resulting in enhanced die life.

In 1969–70, a single Tang dynasty blue-spotted Gongyi sherd was found at Siraf, Iran, the main trading port on the Persian Gulf in the early Islamic period. This is the only known example of Chinese blue-and-white ware, whether low- or high-fired, found in the Middle East from such an early date. The sherd provides direct archaeological evidence for the Indian Ocean trade between China and the Middle East in the ninth century AD. The body paste, clear glaze and blue glaze or pigment were analyzed by thin-section petrography, scanning electron microscopy with energy-dispersive X-ray spectrometry (SEM-EDX) and X-ray fluorescence (XRF). The technological analysis reveals the different steps of the chaîne opératoire: clay mixing, slip and glaze
application, and decoration with the cobalt blue glaze before high-temperature firing. These steps are characteristic of Tang stoneware production at Gongyi in Henan province, China.
The use of cobalt blue pigment as part of a simple spotted decoration scheme on the Gongyi sherd, and its find context within the Middle East, provides evidence for the complex interplay and influence occurring between Chinese and Middle East ceramic industries at this time.
Closely comparable examples of contemporary low-fired earthenware ceramics with cobalt blue decoration on a white tin glaze manufactured within the Middle East also occur within the same assemblage from Siraf.

Presentamos los primeros resultados sobre la naturaleza de los pigmentos utilizados en la decoración de las diferentes manifestaciones cerámicas de la Tambería de Guandacol, oeste de la Provincia de La Rioja. La muestra analizada, mediante Microscopía Electrónica de Barrido y Espectrometría de Energía Dispersiva (MEB-EDS), abarca fragmentos correspondientes a los Estilos Tecnológicos Sanagasta/Angualasto, Inca Provincial, Diaguita Chileno Inca y Aguada; evidencia material asociada fundamentalmente al Periodo de Desarrollos Regionales (ca. 1200-1470 AD) y al de
Dominio Incaico regional (ca. 1470-1533 AD). Los datos obtenidos permiten inferir la existencia de precursores inorgánicos para la confección de pinturas y engobes en los diferentes estilos. Asimismo, se indaga en los procedimientos tecnológicos seguidos durante la etapa de cocción cerámica.

The study of textiles is an open area of scientific research, which for its variety of material components and physical chemical diversity of conditions, makes a field of interest for scientific studies in the cultural heritage field. Archaeological/historical textiles offer the possibility to carry out studies on organic materials such as fibers, adhesion elements, dyes, paper, etc., as well as on inorganic compounds for instance metals, alloys, precious stones and other added ornamentation. That variety of composition, allow to use a combination of analytical techniques to solve the questions coming from the object in an archaeometric research.
One kind of textile object that provides a valuable cultural information because of its linguistic representation employed by its carrier societies, are the flags/banners/emblems, objects made with a nonverbal communication purpose. As long as depending on the use and/or purpose of each object, varies both the materials/techniques used in its production and its iconography (style, color, emblem, shape), its study gives the possibility to extract information through their materials and manufacturing techniques about a temporal-spatial frame, a particular event or a specific character.
The flags/banners have been used since the eleventh century as representative objects of power, hierarchy, social or military organization, or as communicative media. The use of these objects has been spread throughout the world, possibly due to its easy interpretation and/or appropriation by different societies, making it part of their own culture. The flags as symbols of territorial control, using emblems that represent a family, order or army, were introduced to the New World (America) with the arrival of the European conquerors at the end of the fifteenth century. Flags/banners representing the Royal dominion over conquered territories, the Catholic Church and conquistadors’ armies were the first to arrive.
One of those flags that have endured over time, that have an invaluable cultural meaning for both American and Iberian societies, is the so-called Francisco Pizarro’s Banner of Arms. It is a textile object with metal threads decoration over a Royal emblem. According to historical sources, this object was used by Francisco Pizarro in 1532 on the conquest process of Peru, after received the permission by King Charles V to on behalf of him, to conquer the lands of the New World today known as Peru. After Pizarro’s control of the Inca territory, it is believed that Pizarro left his banner on top of the Inca’s Sun’s Temple as symbol of his rule. Centuries later, in the America libertarian campaigns, General Sucre, military at charge of the independence army in Peru, reports have found what he considered the Pizarro’s Banner, sending it to Bogotá as a symbol of victory, being kept since that time until today by the National Museum of Colombia.
Due to historical discrepancies in the different movements of the so-called Pizarro’s Banner of Arms, its real meaning has been under discussion and because of the passage of time its physical condition has suffer deterioration. That is because its scientific study is now an interesting case study to respond to both historical and conservation questions of it.
Through a collaboration with the National Museum of Colombia, a set of 25 samples of so-called Pizarro’s Banner of Arms were collected, covering the various components and areas from the object of study. These samples were subjected to analytical studies for physical and chemical characterization. Microscopic observation, VSEM-EDS analysis, Raman spectroscopy, chromatographic analysis (HPLC-MS, GCMS) and radiocarbon dating were done. Similarly, was sought through a direct in situ physical inspection to the object and through a research into historical sources, adequate information to solve the object’s problems.
Results obtained allowed to identify as silk the textile used in the elaboration of the Banner’s fabric, as well as the use of natural dyes for dyeing the fibers used on the emblem: use of cochineal and brazil wood as a source of red, luteolin plant-based for yellow color, indigotine plant-based for blue, and a mixture of yellow and blue dyes for green were identified. Similarly, the use of animal glue in the manufacturing process and the use of rag paper was evident. The metal threads study from the Banner give a confirmation to a silver core wire gilded with a thin gold sheet, being flattened and entwined with silk threads for their use. Finally, using the radiocarbon results, it was possible to postulate with huge accuracy that the Banner date manufacture was between the XV-XVI century and subject to restoration processes with addition of textiles in modern times. Together with, was evident that the state of degradation of the fabric is due to natural degradation in the silk fibers, having that its color has faded and its mechanical properties decreased, leading to loss of rigidity and disappearance of the physical structure. Similarly, it was clear the original colors of the emblem and highlight problems of detachment of paper due to crystallization of the adhesive. In the same way, was found that the metal threads suffer corrosion by sulfur and detachment of its crystals.
Finally, combining the analytical results and the historical sources data found from the so-called Francisco Pizarro’s Banner of Arms, allows to postulate that its manufacture process was done in Europe employing precious materials to obtain a long-life object with a deep message for its viewers. Also, the data obtained helps to support the possible idea that the object was employed by Francisco Pizarro in the Peru conquest process. However, by the symbols present in the object, its elaboration date and materials, this object its clearly unique in its kind, and the most important, by its linguistic message, does not represent to Francisco Pizarro or his army, meanwhile, represents the Spanish crown. Therefore, instead to be labeled as Francisco Pizarro’s Banner of Arms, it should be called the Colonial Royal Banner of Charles V in the New World.

Las ofrendas de Templo Mayor de Tenochtitlan se caracterizan por su rica variedad de objetos de distintas índoles que destacan por su exuberancia y rareza. En ellas son visibles materiales lapidarios que provienen de diversos sitios del México prehispánico; en la presente investigación se estudiaron los llamados de estilo teotihuacano. Para el entendimiento de cómo se elaboraron los objetos de estilo teotihuacano se utilizó arqueología experimental y por medio de análisis de huellas de manufactura (por medio del SEM) ayudó a dilucidar qué materiales son reliquias Teotihuacanas y cuáles son recreaciones o imitaciones inspiradas en ellas. En la identificación de la materia prima utilizada para elaborar las piezas que se estudiaron fueron necesarios análisis de composición química elemental (por medio de EDS) y molecular (por medio de µ-Raman), que posteriormente sirvió para realizar una comparación minuciosa con todas las muestras que se obtuvieron de diversas fuentes y colecciones. Es a partir de lo anterior que se logró determinar que los objetos de estilo teotihuacano de las ofrendas de Templo Mayor de Tenochtitlan coinciden, no sólo en su manufactura, sino también en la materia prima utilizada en Teotihuacan.

Th e basis for the economic development of Kraków in
the Middle Ages was the city’s involvement in wide-ranging
trade in metals. Back in the 13th century Kraków was a key
player in the sale of Slovakian copper. Th e main route of
exporting that metal passed through the city, from where it
was dispatched to Gdańsk and further by sea to the countries
in Western Europe. Th e merchants of Kraków monopolized
the trade in that precious metal for more than 300 years. They also controlled the sale of Polish lead, exported from the deposits located between Silesia and Kraków via the lead sale centre in the city to Hungary, Bohemia and Germany. Kraków owed its position in the transit trade to a convenient location at the intersection of trading routes and the privileges received from rulers. Th e right to store copper was granted to Kraków in 1306, and the corresponding right with regard to other metals was bestowed upon it before 1335. By his privilege of 1358, King Casimir III the Great confi rmed the right of Kraków to have two scales, one of them being used to weigh metals. Th e existence of such a device in the city back in the 13th century
was confi rmed during the archaeological survey carried out
in Main Market Square (Rynek Główny) in Kraków in the
years 2005–2006. Originally located in a wooden structure,
the scales were housed by a stone and brick building since
the middle of the 14th century.
Metals were not only weighed, but also traded in at the
Great Scales. Th e latter activity was evidenced by the historical
metal items unearthed during the excavations. Apart
from the unique discovery of a huge loaf of lead and an
undamaged slice of copper, the fi nds at the site of the Great
Scales included sections of copper, iron and lead slices, and
a range of smaller fragments pointing to the practice of dividing
pieces of metal intended for retailing. Th e excavation
works also revealed many pieces of metals pointing to
the pursuit of production activities at the Great Scales. As
was confi rmed by metallographic tests, these activities had
most probably been aimed at obtaining silver, and they had
been connected with the silver melting shop situated in the
western part of the building. Th e largest amounts of the
said postproduction scrap metals were found in the deposits
dating back to the 15th and the 16th centuries. It was during
that period that the process of extracting silver from copper
by way of melting the latter with lead became widely popular
across Europe. Th e new method was brought to Kraków
by Jan Th urzo in the second half of the 15th century. It can
be assumed that it was applied during the production activities
the traces of which were discovered at the site of the
former building of the Great Scales. Further research in the
area of metal science will defi nitely contribute to gathering
more knowledge on that matter.

Since welding technology is currently used to assemble the frame of driver's seats, it is important to develop laser welding technology for steel and aluminium. For this reason, the purpose of the present work was to examine the structure and selected properties of aluminium-steel joints using the example of an EN AW-6060 aluminium alloy and DC04 low-alloy steel welded in laser technology. Overlapping joints were made, weld type-following the hole laser welding method-laser beam (LB) using a high power disk laser (TRUMPF TruDisk3302), in which the active medium is a yttrium-aluminium crystal (YAG). Metallographic microstructure investigations were carried out using a light microscope from Carl Zeiss-Observer Z1m, and the weld microstructures were investigated using an SEM Supra 35 microscope, also from Carl Zeiss. The chemical composition analysis in micro-areas was carried out using an X-ray energy dispersion spectrometer from EDAX, which was a part of the SEM Supra 35. The hardness of the substrate material and the welded area was measured following the Vickers method using an FM-ARS 9000 micro hardness tester from Tokyo, Japan. It was found that there is a potential for commercial use of laser welding to make a low-carbon steel-aluminium alloy joint. During the formation of the weld in its microstructure, intermetallic compounds of the FexAly type were created, which significantly reduced the mechanical and plastic properties of the joint. The hardness of the weld created wasabout seven times higher than that of DC04 carbon steel. The choice of laser welding parameters (primarily, laser power and beam speed) significantly impacted the weld structure and properties.

This study is a first approach to glazes of the traditional potter’s village of Sadirac, Gironde. Productions from eight sites from the 14th to the 19th centuries are studied by scanning electron microscopy with energy dispersive X-ray spectrometer (SEM-EDS).
Because of their composition in costly and often inaccessible raw materials unlike clay, looking at glazes can bring information about potter’s work, skills and know-how, besides to inform about social and professional organisation.
The main purpose of this research is to understand raw materials, methods and techniques implemented in conception and recipes of glazing mixture. A first part dealing with physicochemical characterisation of 61 ceramic samples with green glaze will precede the evaluation of the spatial-temporal variations of their compositions.
Results tend to show substantial variations between workshops for all periods. Furthermore, it was possible to correlate some tendencies with deep mutations of this handcraft already describe historically and archeologically.
Key words: Glaze, Sadirac, SEM-EDS, pottery.

Cette recherche porte sur une première approche des glaçures du centre potier de Sadirac, en Gironde. Des productions de huit sites datant du XIVe au XIXe siècle sont étudiées par microscopie électronique à balayage avec spectrométrie de rayons X en dispersion d’énergie (MEB-EDS).
L’étude des glaçures peut nous apporter des informations sur le travail des potiers, leurs techniques et savoir-faire, mais aussi sur l’organisation sociale et professionnelle de cet artisanat. En effet, la glaçure est constituée de matières premières qui sont parfois dispendieuses et inaccessibles localement, contrairement aux argiles.
Cette étude des glaçures du centre potier de Sadirac effectue une première approche des recettes de mélanges glaçurant dans le but de comprendre les matières premières utilisées, ainsi que les techniques et méthodes de fabrication mises en oeuvre. Une première partie concernant la caractérisation physico-chimique de 61 échantillons de céramiques glaçurées vert précédera l’évaluation des variations spatio-temporelles de ces recettes de glaçure.
Les résultats tendent à démontrer une variabilité conséquente au sein des ateliers pour toutes les périodes confondues. De plus, il a été possible de corréler certaines tendances avec des mutations profondes de l’artisanat, déjà entraperçues historiquement et archéologiquement.
Mots-clés : Glaçure, Sadirac, MEB-EDS, poterie.

A cast reliquary cross (enkolpion), found by a treasure hunter using a metal detector in a deserted road (hollow way) near the village of Vitín, became part of the collections of the South Bohemian Museum in České Budějovice in 2016. The following paper describes the Vitín cross, including the alloy from which it was made (brass with lead content and leaded " niello " decoration without silver). The origin of such reliquary crosses is usually sought in Kievan Rus, where they were made in specialized workshops from the 11th to the 13th centuries. In the area of Kievan Rus, especially in the towns of Kiev and Novgorod, we can find precise analogies to the South Bohemian find, which is most likely related to the use of routes that passed through South Bohemia.

Due to the overuse of natural gas and petroleum in Bangladesh, the excessive greenhouse gas (GHG) emission continuously worsens the countries' air quality. To resolve this environmental concern as well as determine the sustainable bioenergy sources, research on biomass for biofuel production has been highlighted recently. Therefore, this study emphasized to identify a novel biomass for solid fuel generation as well as designed a pilot-scale biofuel production scheme. The study endeavoured to characterize the bioenergy properties of a novel wetland moss species, B. dichotomum Hedw., collected from rainforest of Chittagong Hill Tracts (CHT), Bangladesh. Current study also presented the morphological edifice and elemental composition through scanning electron microscopy (SEM)-energy dispersive X-ray (EDX) analysis. Gross and net calorific values of moss were determined through bomb calorimeter by standard method, and they were 10.77 and 9.35 MJ kg −1 , respectively. Moisture content, ash content, volatile matter, fixed carbon, and bulk density were characterized on air-dried basis through standard ASTM methods, and the outcomes were 10.74%, 55.3%, 28.29%, 5.67% and 44.09 kg m −3 , respectively. Other physical bioenergy parameters were biomass characteristics index 3936 kg m −3 , energy density 0.475 GJ m −3 and fuel value index 5.07. Apart from that, experimental results revealed carbon element 56.6%, oxygen content 42.1% on dry weight basis and O/C ratio 0.74 in sample biomass.

Coins were used to maintain the commercial activities on a specific standard. They are significant written sources that enlighten the political, economic, and cultural life of the period they were produced. It is possible to find the coin collections belonging to different periods of Turkish history in museums. One of the important groups of these coins belongs to the Ottoman period. Although there are studies covering the periods of some Ottoman sultans by using advanced analysis techniques in the literature, no scientific study has been carried out covering all periods. The most extensive information that can be found about the coins is from the Ottoman archive and inventory records. In this study, twenty-six Ottoman Empire coins from Sakarya Museum dated between the 14th-19th centuries were evaluated stylistically, physically, and chemically. The non-destructive analysis of scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS) was employed to identify the elemental composition of the coins. The chemical analysis of coins showed the connection between the political situation in the Ottoman Empire and the decline in the value of the money.

Metallurgy in Middle Ages. Raw materials, tools
and facilities in source materials and metallographic
research.
The studies of copper, lead and iron were conducted
to identify old metallurgical processes. Comparatively,
bearing the historical context in mind,
historical raw materials were investigated, coming
from the mediaeval archaeological sites in Krakow,
as well as from the local deposits (Miedzianka) and
from the cargo of the sunken Copper Ship (Miedziowiec).
The archaeological research which was conducted
at the main Market Square in Krakow, unearthed,
inter alia, the Great Scales rooms with many metal
artefacts inside, bearing evidence of production
of metal and preparing it for merchandising. The
establishment of the Great Scales was connected
directly with the right to store copper, which Krakow
obtained in 1306. Copper from the mines and
smelters in Spisz, via Krakow and Toruń it got to
Gdańsk, and from there, by sea, to Flanders.
A lot can be learnt from city records, especially the
account books, about functioning of the municipal
scales in Krakow used for weighing raw materials
(copper, lead and iron) and the local melting shop.
In the sources there is a note preserved regarding
expenses for tools and facilities for the Great
Scales, for repairing the axes for cutting lead and
purchasing the new ones. Also, under the entry of
Purchases for the Great Scales there are expenses
for copper, lead and white iron (ferrum album). The
reconstruction of the process as well as the tools
used can be done based on G. Agricola De re metallica
libri XII (1556).

The precious metals of the early medieval period were the same as those of today. Knowing their purity was essential, which means that assaying and refining were of great importance. Touchstones have been used to assess the quality of precious metals since antiquity. Stone artefacts initially identified as whetstones were unearthed in two of the most prestigious chamber graves discovered at the cemetery in Ciepłe. Traces of precious and nonferrous metals on the surface of the object from Grave 42 proved that this artefact was a touchstone. It is probable that the phyllite stone from the other grave served the same purpose. Tools of this type are often found in high-prestige burials in Europe, in some cases together with balance scales and weights, which suggests that the individuals in whose graves they were deposited had access to precious metals. Therefore interpreting touchstones as a reliable indicator of the high social standing of the deceased seems entirely reasonable.

Paper touches on an issue of five pottery sherds from site 8 in Szczepanki with suspicious and exceptionally repetitive, regular and suggestive dark patterns on their surfaces. To verify whether these patters are dyed or are the effect of natural processes method of scanning electron microscopy SEM and analysis of chemical composition using coupled with microscope energy dispersion microprobe has been chosen. Concomitancing frequencies growths of carbon, iron and calcium alike found on darkened surfaces combined with characteristic crack grid typical for dried out substances and granulation looking just like grains of sand show distinctly the occurence of formerly humid silt fraction with organic-mineral admixture, which must have been put on intentionally on sherds' surface. Author in her digressions sees both stylistic and semantic similarities mainly in the rock art of southern Finland, which is being linked to contemporary with Zedmar Culture Comb Ware Culture, but also in some Trypolye Culture finds from as well. In the context of dyes manufacturing technology analogies with both Funnelbeaker Culture and Neman Culture has been noticed. Implemented research method has interdisciplinary features to investigate suspicious sherds in the most holistic way possible. The very first proofs of painting pottery with organic-mineral dyes and figurative motives in Zedmar Culture has been provided. Paper also brings a bunch of new data regarding relations of Zedmar Culture with Paraneolithic and Neolithic cultures. Meanwhile, it confirms V. I. Timofeev's opinion on Zedmar Culture being a hybrid between the two worlds.

Keywords: Raman SEM–EDS Inks Jarosite Elderberry Surprising discoveries can happen while analyzing library materials. This paper presents four case studies focusing on four artifacts of different ages and provenances, all analyzed and studied at the Istituto Centrale per il Restauro e la Conservazione del Patrimonio Archivistico e Librario (Icrcpal). The common denominator amongst the case studies presented in this work, lies in the need for a strong intercon-nection between the analysis of biological issues and chemical data. The interplay between the two complementary approaches is paramount for the correct interpretation of the status of the material under examination as, as will be shown in the following case studies, chemical data could find an interpretation only in the face of biological observations and vice versa. The first case we here present, deals with two parchment codices that have been found in 2008 during a fishing expedition in the Canale di Sicilia. At that time a deep-sea fishing boat belonging to the fleet of Mazara del Vallo caught in its nets, two artifacts, leading to the first discovery of library materials in the deep sea. The Scanning Electron Microscopy and Energy Dispersive Spectroscopy (SEM/EDS) analyses allowed for the creation of a com-positional map of the surface of the samples, where several microscopic encrusting sea organisms and biogenic materials were also observed. Almost nothing of the original structure of the parchment (of which the object is presumably made) could be recognized at SEM. The absence of the typical collagen features was confirmed by Raman analyses that could only collect spectra of an isoprenic-type polymer of putative biogenic origin. The second case deals with fragments of medieval manuscripts that were found in 2007 buried in the walls of the Great Mosque of Sana'a in Yemen. An outstanding discovery regarded the dark brown inks used on a Qur'ānic fragment attributed to the 10th century. SEM micrographs disclosed the presence of red blood cells mixed to ink components. The inks were also investigated with Raman spectroscopy. The third case study is the book " Libretto di appunti e memorie del Padre Francesco Zazzera " , dated 17th century that presented a peculiar modification of the black ink that appeared to be faded and turned to a white-yellowish color. Raman and SEM analyses recognized and documented a biogenic formation of jarosite on top of the ink. It was possible to remove the jarosite layer and to recover the original black ink, thus allowing an easier reading of the text. The fourth and last case analyzed and presented in this paper consists of the measurements on the invaluable Codex Purpureus Rossanensis dated 6th century. Raman spectroscopy here allowed the demonstration of the use of an elderberry lake to obtain a mauve color. This is the first experimental evidence of the use of that particular dye in such an ancient illuminated manuscript. A sort of archeological discovery was also done on this codex with respect to the past misfortunes that occurred to it; by simply observing some traces we were able to support some intriguing hypothesis on its history and vicissitudes.

This paper looks at the development of the bottle glass industry in England. The production of bottles is considered from both a typological perspective and through the chemical composition of the glass used. Samples of bottles and bottle production debris from many different production sites have been analysed to determine their chemical composition. The changes in the social organisation of the industry are discussed in relation to the changing materials and technologies employed in bottle production.