SEM-EDX and FTIR analysis of archaeological ceramic potteries from southern Italy

Microscopy ◽  
2020 ◽  
Vol 69 (6) ◽  
pp. 371-380
Author(s):  
Tania Dey ◽  
Joseph Coleman Carter ◽  
Keith Swift
Keyword(s):  
Firing Temperature ◽  
Southern Italy ◽  
Raw Materials ◽  
Silica Nanoparticle ◽  
Glassy Matrix ◽  
Processing Temperature ◽  
Valuable Insight ◽  
Sem Image ◽  
Three Samples ◽  
Two Samples

Abstract Sherds of ancient ceramics potteries, dating back to the seventh century BC and excavated from southern Italy, were analyzed in terms of microstructure and porosity (SEM), elemental composition (EDX), chemical bonding and mineralogical components (FTIR) in order to establish correlation with firing temperature, firing condition and provenance. Si/Al ratio from EDX analysis showed three major categories of raw materials (illite/montmorillonite, kaolinite and mullite), suggesting difference in provenance. Uniformly sized silica nanoparticle (0.7 μm diameter) and trace amount of silver are being reported for the first time in one sample. Anorthite mineral and quartz inclusion was detected by FTIR in certain samples. All samples showed a prominent band for Si-O stretching, which shifted from 1062 cm−1, broadened and appeared as doublet, relative to processing temperature. FTIR results proved incomplete dihydroxylation and undissociated carbonate in three samples, indicating a firing temperature of 700–800°C, whereas other samples were fired above 900°C. Only one sample among these three showed bloating pores in between interconnecting glassy matrix in SEM image, indicating a firing temperature of 1100–1200°C. The absence of magnetite along with significant Fe and Mn content indicated the formation of jacobsite, an iron manganese spinel complex, MnFe2O4, which is responsible for the black gloss effect in two particular samples and can be further confirmed by XRD. The presence of numerous small pores in SEM image of one of these two samples (1.2 μm diameter) was indicative of extended vitrification at higher temperature than the other one. However, magnetite was responsible for black gloss effect in two other samples, proving difference in provenance. Therefore, SEM-EDX and FTIR results can offer valuable insight into the firing conditions, gloss decoration and provenance of ancient ceramic potteries.

scholarly journals Chemotypical diversity of Mentha longifolia L. oil

2021 ◽  
pp. 130-139
Author(s):  
O. M. Shevchuk ◽  
S. A. Feskov ◽  
N. A. Bagrikova ◽  
I. V. Tania
Keyword(s):  
Essential Oil ◽  
Mass Fraction ◽  
Raw Materials ◽  
Three Samples ◽  
Two Samples ◽  
Mentha Longifolia ◽  
Wet Weight

The article presents data on the content and composition of the essential oil of Mentha longifolia (L.) L. plants growing in natural phytocenoses on the territory of Crimea and Abkhazia. It was found that dry raw materials in two samples from natural phytocenoses of Crimea contain 1.27 and 1.76% of essential oil per wet weight, three samples from phytocenoses of Abkhazia contain less essential oil - 0.68, 0.98 and 1.19 %. About 60 components have been identified. Two new chemotypes were identified for Crimea: carvone-piperitone (mass fraction of carvone is 66.65%, piperitone oxide - 14.37%) and piperitone-sabinene (mass fraction of piperitone oxide - 55.19% and cis-sabinene hydrate - 23.51%), and two for Abkhazia: terpene-caryophyllene (α-terpinyl acetate - 51.48%;  β-caryophyllene - 9.26%), piperitone-non-petalactone (piperitone oxide - 46.29%;  nepetalactone 4aa, 7a, 7aa - 34.85%). These Mentha longifolia chemotypes are promising for use in the food, chemical, pharmaceutical and perfume industries. 

scholarly journals Elemental Characterization of Ciders and Other Low-Percentage Alcoholic Beverages Available on the Polish Market

Molecules ◽  
2021 ◽  
Vol 26 (8) ◽  
pp. 2186
Author(s):  
Magdalena Gajek ◽  
Aleksandra Pawlaczyk ◽  
Piotr Wysocki ◽  
Malgorzata I. Szynkowska-Jozwik
Keyword(s):  
Raw Materials ◽  
Statistical Tests ◽  
Analytical Data ◽  
Alcoholic Beverages ◽  
Data Set ◽  
Apple Variety ◽  
Three Samples ◽  
Two Samples ◽  
Elemental Fingerprint ◽  
The Impact

Seventy-three samples of alcoholic beverages and juices that were purchased on the Polish market and home-made were analyzed for their elemental profiles. The levels of 23 metals were determined by ICP-MS (Ag, Ba, Bi, Cd, Co, Cr, Li, Mn, Ni, Pb, Sr and Tl), ICP-OES (Al, B, Ca, Cu, Fe, K, Mg, Na, Ti and Zn) and CVAAS (Hg) techniques in twenty-five samples of ciders widely available on the Polish market; six samples of home-made ciders; two samples of juices used in the production of these ciders; and forty samples of low-percentage, flavored alcoholic beverages based on beer. The gathered analytical data confirmed that the final elemental fingerprint of a product is affected by the elemental fingerprint of the ingredients used (apple variety) as well as the technology and equipment used by the producer, and in the case of commercial ciders, also the impact of type of the packaging used was proven. These factors are specific to each producer and the influence of the mentioned above parameters was revealed as a result of the performed analysis. Additionally, the inclusion of the home-made ciders in the data set helped us to understand the potential origin of some elements, from the raw materials to the final products. The applied statistical tests revealed (Kruskal–Wallis and ANOVA) the existence of statistically significant differences in the concentration of the following metals: Ag, Al, B, Bi, Co, Cr, Cu, Fe, K, Li, Mg, Na, Ni, Ti and Zn in terms of the type of cider origin (commercial and home-made). In turn, for different packaging (can or bottle) within one brand of commercial cider, the existence of statistically significant differences for Cu, Mn and Na was proved. The concentrations of all determined elements in the commercial cider from the Polish market and home-made cider samples can be considered as nontoxic, because the measured levels of elements indicated in the regulations were lower than the allowable limits. Moreover, the obtained results can be treated as preliminary for the potential authentication of products in order to distinguish the home-made (fake) from the authentic products, especially for premium-class alcoholic beverages.

scholarly journals Biosystematic Study on Some Egyptian Species of Astragalus L. (Fabaceae)

Agriculture ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 125
Author(s):  
Monier M. Abd El-Ghani ◽  
Ashraf S. A. El-Sayed ◽  
Ahmed Moubarak ◽  
Rabab Rashad ◽  
Hala Nosier ◽  
...  
Keyword(s):  
Genetic Relationships ◽  
Dna Barcode ◽  
Plant Morphology ◽  
Its Region ◽  
Its2 Region ◽  
Whole Plant ◽  
Three Samples ◽  
Two Samples ◽  
Region 10 ◽  
Unique Banding Pattern

Astragalus L. is one of the largest angiosperm complex genera that belongs to the family Fabaceae, subfamily Papilionoideae or Faboideae under the subtribe Astragalinae of the tribe Galegeae. The current study includes the whole plant morphology, DNA barcode (ITS2), and molecular marker (SCoT). Ten taxa representing four species of Astragalus were collected from different localities in Egypt during the period from February 2018 to May 2019. Morphologically, identification and classification of collected Astragalus plants occurred by utilizing the light microscope, regarding the taxonomic revisions of the reference collected Astragalus specimens in other Egyptian Herbaria. For molecular validation, ten SCoT primers were used in this study, producing a unique banding pattern to differentiate between ten samples of Astragalus taxa which generated 212 DNA fragments with an average of 12.2 bands per 10 Astragalus samples, with 8 to 37 fragments per primer. The 212 fragments amplified were distributed as 2 monomorphic bands, 27 polymorphic without unique bands, 183 unique bands (210 Polymorphic with unique bands), and ITS2 gene sequence was showed as the optimal barcode for identifying Astragalus L. using BLAST searched on NCBI database, and afterward, analyzing the chromatogram for ITS region, 10 samples have been identified as two samples representing A. hauarensis, four samples representing A. sieberi, three samples representing A. spinosus and one sample representing A. vogelii. Based on the ITS barcode, A. hauarensis RMG1, A. hauarensis RMG2, A. sieberi RMG1, A. sieberi RMG2, A. sieberi RMG3, A. sieberi RMG4, A. spinosus RMG1, A. spinosus RMG2, A. spinosus RMG3, A. vogelii RMG were deposited into GenBank with accession # MT367587.1, MT367591.1, MT367593.1, MT367585.1, MT367586.1, MT367588.1, MT160347.1, MT367590.1, MT367589.1, MT367592.1, respectively. These results indicated the efficiency of SCoT markers and ITS2 region in identifying and determining genetic relationships between Astragalus species.

scholarly journals A Comparison of the Composition of Selected Commercial Sandalwood Oils with the International Standard

Molecules ◽  
2021 ◽  
Vol 26 (8) ◽  
pp. 2249
Author(s):  
Malgorzata Kucharska ◽  
Barbara Frydrych ◽  
Wiktor Wesolowski ◽  
Jadwiga A. Szymanska ◽  
Anna Kilanowicz
Keyword(s):  
Mass Spectrometry Analysis ◽  
Santalum Album ◽  
Benzyl Benzoate ◽  
Spectrometry Analysis ◽  
Correct Information ◽  
Three Samples ◽  
Two Samples ◽  
High Street ◽  
Chromatographic Profile ◽  
Sandalwood Oil

Sandalwood oils are highly desired but expensive, and hence many counterfeit oils are sold in high street shops. The study aimed to determine the content of oils sold under the name sandalwood oil and then compare their chromatographic profile and α- and β santalol content with the requirements of ISO 3518:2002. Gas chromatography with mass spectrometry analysis found that none of the six tested “sandalwood” oils met the ISO standard, especially in terms of α-santalol content. Only one sample was found to contain both α- and β-santalol, characteristic of Santalum album. In three samples, valerianol, elemol, eudesmol isomers, and caryophyllene dominated, indicating the presence of Amyris balsamifera oil. Another two oil samples were found to be synthetic mixtures: benzyl benzoate predominating in one, and synthetic alcohols, such as javanol, polysantol and ebanol, in the other. The product label only gave correct information in three cases: one sample containing Santalum album oil and two samples containing Amyris balsamifera oil. The synthetic samples described as 100% natural essential oil from sandalwood are particularly dangerous and misleading to the consumer. Moreover, the toxicological properties of javanol, polysantol and ebanol, for example, are unknown.

scholarly journals Mineralogical Characterization and Firing Temperature Delineation on Minoan Pottery, Focusing on the Application of Micro-Raman Spectroscopy

Heritage ◽  
2019 ◽  
Vol 2 (3) ◽  
pp. 2652-2664 ◽  
Author(s):  
E. Grammatikakis ◽  
Kyriakidis ◽  
D. Demadis ◽  
Cabeza Diaz ◽  
Leon-Reina
Keyword(s):  
Bronze Age ◽  
Firing Temperature ◽  
Raw Materials ◽  
Morphological Characteristics ◽  
Ceramic Technology ◽  
Phase Identification ◽  
Mineralogical Characterization ◽  
Analytical Protocol ◽  
Crucial Information ◽  
Analytical Tools

Ceramic objects in whole or in fragments usually account for the majority of findings in an archaeological excavation. Thus, through examination of the values these items bear, it is possible to extract important information regarding raw materials provenance and ceramic technology. For this purpose, either traditional examination protocols could be followed, focusing on the macroscopic/morphological characteristics of the ancient object, or more sophisticated physicochemical techniques are employed. Nevertheless, there are cases where, due to the uniqueness and the significance of an object of archaeological value, sampling is impossible. Then, the available analytical tools are extremely limited, especially when molecular information and mineral phase identification is required. In this context, the results acquired from a multiphase clay ceramic dated on Early Neopalatioal period ΜΜΙΙΙΑLMIA (1750 B.C.E.–1490 B.C.E.), from the Minoan Bronze Age site at Philioremos (Crete, Greece) through the application of Raman confocal spectroscopy, a nondestructive/ noninvasive method are reported. The spectroscopic results are confirmed through the application of Xray microdiffraction and scanning electron microscopy coupled with energy dispersive Xray spectrometry. Moreover, it is demonstrated how it is made possible through the application of microRaman (μRaman) spectroscopy to examine and collect crucial information from very small inclusions in the ceramic fabric. The aim of this approach is to develop an analytical protocol based on μRaman spectroscopy, for extracting firing temperature information from other ceramic finds (figurines) where due to their uniqueness sampling and analyses through other techniques is not possible. This information can lead to dating but also to firing kiln technology extrapolations that are very significant in archaeology.

Bentonite granulates as a seals for mobile flood barriers

2021 ◽  
Vol 11 (4) ◽  
pp. 16-23
Author(s):  
Piotr Wrona ◽  
Wojciech Panna ◽  
Stanisław Lipiński ◽  
Maciej Woźniak
Keyword(s):  
Comparative Analysis ◽  
Size Distribution ◽  
Raw Materials ◽  
Test Stand ◽  
Three Samples

Bentonites and other smectite raw materials are widely used in many industries. The authors of the study analyzed the suitability of swelling granulates for their use as a seals in mobile flood barriers. For this purpose, a comparative analysis of the swelling and granulation parameters of three samples available on the market was performed. This results was compared with a macroscopic swelling test, which was realized on the specially prepared test stand. The carried out research shows that not only the content of the swelling minerals – mainly smectite – affect on the sealing of the system, but also they are determine by granules size distribution and the type of smectite.

Magnetic study of Fe3O4/Ag nanoparticles

2018 ◽  
Vol 83 (1) ◽  
pp. 10402
Author(s):  
Janusz Typek ◽  
Nikos Guskos ◽  
Grzegorz Zolnierkiewicz ◽  
Zofia Lendzion-Bielun ◽  
Anna Pachla ◽  
...  
Keyword(s):  
Antibacterial Properties ◽  
Blocking Temperature ◽  
Precipitation Method ◽  
Magnetic Clusters ◽  
Mass Ratio ◽  
Three Samples ◽  
Two Samples ◽  
Magnetic Resonance Technique ◽  
Silver Nps ◽  
Multi Mode

Nanocomposites of Fe3O4 nanoparticles (NPs) impregnated with silver NPs display antibacterial properties and may be used in water treatment as disinfection agent. Three samples were synthesized: Fe3O4 NPs obtained by the precipitation method and additionally two samples with added silver NPs with mass ratio of Ag:Fe3O4 equal to 1:100 and 2:100. Magnetic properties of these samples were studied by SQUID magnetometry (in temperature range 2–300 K and magnetic fields up to 70 kG) and magnetic resonance technique at RT. Temperature dependence of dc susceptibility revealed the blocking temperature close to RT in all three samples and allowed to determine the presence of single or multi-mode distribution of NP sizes in a particular sample. Isothermal magnetisation measurements showed that the presence of silver NPs, especially those with smaller sizes, decreases the saturation magnetisation. The shape of ferromagnetic loop registered at T = 2 K was used to discuss the sizes of NP magnetic clusters in our samples. Conclusions obtained from analysis of the ferromagnetic resonance spectra were consistent with the propositions based on the magnetometric studies.

The Influence of Ferrous Metallurgy Waste in the Aktobe Region on the Frost Resistance of Ceramic Bricks Based on Low-Melting Clay

2021 ◽  
Vol 887 ◽  
pp. 453-459
Author(s):  
A.K. Kairakbaev ◽  
E. S. Abdrakhimova ◽  
V.Z. Abdrakhimov
Keyword(s):  
Liquid Phase ◽  
Moisture Content ◽  
Firing Temperature ◽  
Frost Resistance ◽  
Glass Phase ◽  
Raw Materials ◽  
Residual Moisture ◽  
Chromite Ore ◽  
Alkali Oxides ◽  
Pass Through

The research objective is studying the effect of tailing slurry of chromite ore beneficiation on the phase composition and frost resistance of ceramic bricks obtained based on low-melting clay. For the study, two compositions were taken, % wt.: 1) the optimal composition ─ low-melting clay of the Ilek deposit - 70, tailing slurry of chromite ore beneficiation, 2) the reference composition ─ low-melting clay of the Ilek deposit - 100. Raw materials were crushed to pass through a sieve No. 1.0 mm; then, the components were thoroughly mixed. The bricks were prepared by melting at a batch moisture content of 22 %. The mold bricks were dried to a residual moisture content of 5 % max. The dried bricks were fired at temperatures, оС: 950 (the glass phase emergence), and 1,050 (the final brick firing temperature). The increased content of iron oxide (Fe2O3=12.3 %) and alkali oxides (R2O=3.2 %) in the tailing slurry of chromite ore beneficiation contributed to the liquid phase emergence at 950 оС. Colorless, yellowish, and brown glasses with refractive indices N within 1.50-1.54, forming as a result of melting of spars and mixed-layer clayey formations, were observed under the microscope in the studied prototypes of composition No. 1 at a firing temperature of 950 °C. In the composition No. 2, a liquid phase also emerges, but in smaller quantities. Adding tailing slurry of chromite ore beneficiation to ceramic masses contributes to the formation of anorthite and glass phase in prototypes based on low-melting clay at a firing temperature of 950 °C. An increase in the firing temperature to 1,050 °C increases the content of the glass phase and anorthite, which significantly improves the frost resistance of ceramic bricks.

scholarly journals The Effect of Weathering on Salt Release from Coal Mine Spoils

Minerals ◽  
2019 ◽  
Vol 9 (12) ◽  
pp. 760
Author(s):  
Melinda Hilton ◽  
Mandana Shaygan ◽  
Neil McIntyre ◽  
Thomas Baumgartl ◽  
Mansour Edraki
Keyword(s):  
Particle Size ◽  
Coal Mine ◽  
Chemical Weathering ◽  
Physical Weathering ◽  
Particle Size Fractions ◽  
Mine Spoils ◽  
Weathering Processes ◽  
Three Samples ◽  
Two Samples ◽  
Physical And Chemical

Coal mine spoils have the potential to create environmental impacts, such as salt load to surrounding environments, particularly when exposed to weathering processes. This study was conducted to understand the effect of physical and chemical weathering on the magnitude, rate, and dynamics of salt release from different coal mine spoils. Five spoil samples from three mines in Queensland were sieved to three different particle size fractions (<2 mm, 2–6 mm, and >6 mm). Two samples were dispersive spoils, and three samples were nondispersive spoils. The spoils were subjected to seven wet–dry cycles, where the samples were periodically leached with deionised water. The rate, magnitude, and dynamics of solutes released from spoils were spoil specific. One set of spoils did not show any evidence of weathering, but initially had higher accumulation of salts. In contrast, broad oxidative weathering occurred in another set of spoils; this led to acid generation and resulted in physical weathering, promoting adsorption–desorption and dissolution and, thus, a greater release of salts. This study indicated that the rate and magnitude of salt release decreased with increasing particle size. Nevertheless, when the spoil is dispersive, the degree of weathering manages salt release irrespective of initial particle size. This study revealed that the long-term salt release from spoils is not only governed by geochemistry, weathering degree, and particle size but also controlled by the water/rock ratio and hydrological conditions of spoils.

scholarly journals A Study of the Micropore Structure of Carbonized Rayon Yarn by Nitrogen Adsorption and Nonane Pre-Adsorption

1985 ◽  
Vol 2 (2) ◽  
pp. 89-95 ◽  
Author(s):  
J. N. Bohra ◽  
K. S. W. Sing
Keyword(s):  
External Surface ◽  
Nitrogen Adsorption ◽  
The Other ◽  
Adsorption Method ◽  
Micropore Structure ◽  
Surface Areas ◽  
Three Samples ◽  
Two Samples ◽  
Before And After ◽  
Gain Access

Adsorption isotherms of nitrogen have been determined at 77 K on three samples of carbonized rayon yarn, both before and after the pre-adsorption of n-nonane. In their original state the three samples were all highly microporous. Application of the αs-method of isotherm analysis reveals that their micropore volumes were 0·17–0·19 cm3g−1 and their external surface areas 20–27 m2g−1 (the corresponding BET areas being 427–483 m2g−1). Nonane pre-adsorption resulted in blockage of the entire micropore structure only in the case of one sample: micropore volumes ∼0·1 cm3g−1 were still available for nitrogen adsorption in the other two samples. It appears that nitrogen molecules were able to gain access to some parts of these micropore structures through wider pore entrances which were not completely blocked by the pre-adsorbed nonane. The work has shown that the nonane pre-adsorption method requires further investigation before it can be used with confidence for the assessment of microporosity.

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