Energy Dispersive X-ray Fluorescence Analysis Research Articles

Forensic Elemental Analysis of Five Rupee and One Pound Coin with EDXRF Technique

Energy dispersive X-ray Fluorescence (EDXRF) technique using synchrotron radiation has been employed for elemental analysis of one pound and five rupees coins of two different countries- the UK and India. Total number of 12 coins - 4 one pound and 8 five rupees coin were analysed. A Peltier cooled Vortex solid state detector (SII Nano Technology, USA) having energy resolution of 138 eV at 5.96 keV X-rays was employed for the present analysis. A Peltier cooled Vortex solid state detector (SII Nano Technology, USA) having energy resolution of 138 eV at 5.96 keV X-rays was employed for the present analysis. The investigations were carried out to determine the similarities between the elemental composition and structure of coins. The major elements Cu, Ni, Fe, Cr and traces of two elements Mn and Mo were found during analysis. One of the elements i.e. Cu was found as primary major element in most of the coins. Two other elements Fe and Cr are also found as major element in 2 five rupees coins. Fe was generally considered as cheap metal composition in comparison to Cu. Besides these traces of Mo, S, Ca and Si were also observed whose compositional amount found very low (below 1%). The present study confirms the favorable economic conditions of two countries during their minting time. The XRF spectra and graphical representation of elemental concentration also helps to identify the similarities in structure and composition of coins. Results of present analysis of different types of coins are found in good agreement with standard composition and also with each other. The EDXRF analysis shows its effectiveness in forensic science without alteration of precious samples. Forensic analysis of such coins using Synchrotron radiation is very helpful in archeological study.

A provenance study on the ceramics excavated at the Varzaneh Plain, central Iran

Forty-six ceramic shards from the Early Bronze Age (EBA) archaeological site of Tappeh Gabri (the archaeological site 013), dated back to the latter half of the third millennium BCE and located at the Varzaneh Plain, central Iran, were studied using micro energy dispersive X-ray fluorescence (µ-EDXRF) and petrographic analysis. The precision and accuracy of quantitative data obtained by µ-EDXRF were tested using a series of geological certified reference materials (CRM). The expanded uncertainty and the Mantel test on data obtained by µ-EDXRF showed accurate and precise quantitative µ-EDXRF estimation of elements present in the CRMs above their quantification limit. We show that the majority of the ceramics at the Varzaneh Plain is most probably local product. Discussions prompted collecting further compositional data and performing petrographic investigation from the ceramic shards from southern and south-western Iran in order to shed light on the origin of the ceramic shards excavated at the Varzaneh Plain.

X-Ray Fluorescence Measurements of Elements in High Matrix Solution Using Solid Substrate Having Nanoporus Structure

X-ray fluorescence (XRF) analysis can determine directly and non-destructively the elemental composition of various materials such as solid samples and water. For multi-elemental analysis of low volume (sub-milliliter levels) solution, XRF analysis combining with a droplet method is effective. In general, a dried droplet on a filter paper is analyzed in the droplet method. For measurements on high matrix solution, however, the sensitivity is reduced, resulting in large spread of values. In this study, to improve the sensitivity and repeatability of determination values of elements in high matrix solution by an XRF analysis with a droplet method, a silicon substrate having nanoporous structure was used instead of conventional filter paper. Two methods ((i) anodic etching using a hydrofluoric acid, (ii) metal-assisted chemical etching using gold and silver particles) were applied to silicon for introducing nanoporous structure on the surface of silicon. Different nanoporous structures were formed on the surface reflecting each etching condition. In the case of anodic etching, the silicon surface had spongy nanoporous structure. A dried residue containing 1 mg of the element was prepared on the etched silicon to investigate the effect of the nanoporous structure on the thickness and area of the dried residue. The size, shape and thickness of the dried residue were affected by the surface morphology of the silicon prepared by various etching conditions. Among them, the dried residue formed on anodic etched porous silicon was most circular and uniform. As compared with a flat silicon, the sensitivity and repeatability of energy dispersive XRF analysis by droplet method were improved by using a substrate having nanoporous structure. Especially, the intensity of Mg Kα increased by 11 times, and relative standard deviation (n = 5) of X-ray intensity of Mg Kα decreased by 1/5.

Field determination of trace concentrations of hazardous metals in waters by portable EDXRF.

A new effective method has been developed for field determination of trace concentrations of cadmium, arsenic, zinc, copper, nickel, chromium, and lead in waters (e.g., surface and wastewater) using an energy dispersive X-ray fluorescence (EDXRF) analyzer. Trace concentrations cannot be determined by EDXRF without preconcentration. Agar was used for the preconcentration of these potentially toxic elements (PTE). Metals are trapped in the three-dimensional network of agar gel. Subsequent swelling of the gel leads to more effective preconcentration. The swollen gels with PTE were analyzed by a portable energy dispersive X-ray fluorescence analyzer Delta Professional X (pXRF). The preconcentration factors for each PTE were determined. With pXRF, the detection limits were 7, 5, 6, 7, 9, 47, and 22 µg/L for Cr, Ni, Cu, Zn, As, Cd, and Pb, respectively. A reference material was used to assess the methodology performance, and it has a very good agreement. The optimized and verified methodology was tested in practice at the special chemical unit of the Fire Rescue Service of the Czech Republic. PTE were determined by pXRF in a mobile chemical laboratory in field analysis. The measured values were compared with those determined via inductively coupled plasma mass spectrometry (ICP-MS) and were in good agreement. Our method was applied to real wastewater samples collected during after a fire of accumulation batteries of domestic photovoltaic power plants, allowing accurate real-time estimation of PTE concentrations. Obtaining reliable data during an ecological accident has a very important role in minimizing the subsequent environmental impact of the accident.

Bismuth-gold nanohybrid based nano photosensitizer to combat antimicrobial resistance

Antimicrobial resistance (AMR) leads to a decrease in the adequacy of antimicrobial agents and an increase in the rate of adverse effects and mortality. The main objective of this project is to investigate the synergistic effect of BiAu@NCLin-T1 and its substructures as an antimicrobial photodynamic therapy (aPDT) agent to combat microbial resistance. In addition, the effect of photothermal therapy (PTT) on some of the designed nanostructures at a temperature of 40 °C was also tested. The antimicrobial test was carried out using the growth curve method against Escherichia coli and Staphylococcus aureus. Computational methods were used to investigate the stability and entropy of oligonucleotide sequence structures. Various analyses were performed to identify the nanostructures, including Ultraviolet–visible (UV–vis) spectroscopy, Fourier-transform infrared spectroscopy (FTIR), dynamic light scattering (DLS), transmission electron microscopy (TEM), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray analysis (EDS) and fluorescence analysis. The BiAu@NCLin-T1 appeared the significant aPDT impact against the gram-negative E.coli strain at two distinctive oligonucleotide concentrations (1, and 1.5 micromolar (µM)). Based on the results, the outlined nanostructures can act as a photosensitizer (PS), a photothermal treatment (PTT) agent, and an antimicrobial agent to combat resistant bacteria.

Properties of biocoal briquettes from mesoporous coals and rice husk and their effects on environmental pollution

This work assessed some properties and effects of biocoal briquettes on environmental pollution compared with utilising coal alone. A mixture of coal fines and rice husks was prepared, with cassava starch gel as a binder, before compaction in a briquetting machine and drying with a solar dryer. Samples of the coal fines, rice husk, cassava flour and briquettes were analysed for their elemental and oxide concentrations via an energy-dispersive X-ray fluorescence analyser. The heat fuels were analysed for their thermal behaviour via thermogravimetric analyser (TGA), whereas the specific surface area, pore size and pore volume were determined using a Brunner–Emmett–Teller (BET) analyser. The conversion of the tested coals to biocoal briquettes resulted in a reduction in the level of arsenic in the briquettes. Additionally, the sulphur level decreased from 1.96 to 1.11% in the Okobo-Enjema briquettes and from 1.78 to 0.90% in the Onyeama briquettes. However, the levels of manganese increased from 0.04 to 0.22% in the Okobo-Enjema briquettes and from 0.04 to 0.21% in the Onyeama briquettes. Thermogravimetric analysis at different heating rates revealed that derivative weight loss increased with increasing heating rate, from 4.4% at 10 °C/min to 5.5% at 20 °C/min. BET analysis revealed that the briquettes had larger pore diameters, volumes and specific surface areas than did the coal samples. The coal samples have greater propensity to pollute the environment as the amount of potentially hazardous elements in the samples is greater than in their biocoal briquettes.

New data about the provenance of the Early Eneolithic copper artefacts from western Lesser Poland

Abstract The Early Eneolithic period in Lesser Poland is represented by the Lublin-Volhynian culture and the Wyciąże-Złotniki group. For both of them, the main cultural references were the Middle Copper Age groups from the Carpathian Basin (the Bodrogkeresztúr, the Hunyadihalom-Lažňany, the Balaton-Lasinja cultures, as well as the Ludanice, and the Bajč-Retz-Gajary groups). One of the most important indicators of the Transcarpathian influence was the use of various copper objects by local communities and their deposition in graves. A set of seventeen objects, mostly from well-dated grave contexts, was analysed to establish the provenance of the copper artefacts used in western Lesser Poland. This set included artefacts discovered in Złota Grodzisko I and Grodzisko II, Książnice 2, Koniecmosty, Kraków-Wyciąże 5 and Kraków-Cło 7. Energy dispersive X-ray fluorescence analysis was used to study the chemical compositions, while lead isotope ratios were determined using a inductively coupled plasma mass spectrometer (HR-MC-ICP-MS). In addition, some of the objects were visually inspected under a digital microscope to determine how they were made and used. As a result of this analytical programme, it was possible to establish that both Lesser Poland groups used the same copper distribution networks. Initially (c. 4050–3950 BC), the copper originated from the mines in Serbia that at the time were controlled, as suggested in the literature, by the peoples of the Bodrogkeresztúr culture, and also from the mines in the Slovak ore Mountains, linked to the Ludanice group. It appears, however, that from c. 3950 BC onwards, the only source of metal for the production of copper objects used by the inhabitants of western Lesser Poland were the mines located in the Slovak Ore Mountains. This research also suggested that, while around 3950–3800 BC, there was a marked regression in the production and use of copper artefacts in the Carpathian Basin, in the area of western Lesser Poland there was an increase in the use and, most likely, local production of original copper jewellery.

Eco-friendly synthesis and antibacterial potential of chitosan crosslinked-EDTA silver nanocomposite (CCESN)

This study presents a novel and eco-friendly approach for synthesizing silver nanocomposite at room temperature. The method utilizes chitosan derived from snail (Archachatina marginata) shell waste crosslinked with EDTA as a combined reducing and capping agent. The existence of silver nanoparticles in the composite was confirmed by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffractometry (XRD), energy dispersive X-ray (EDX), energy dispersive X-ray fluorescence (EDXRF) and thermogravimetric analysis (TGA). The TEM, SEM, XRD, and analyses revealed that the silver nanoparticle has a face-centered cubic structure with an average size of 45.30 nm respectively. EDX and EDXRF showed characteristic silver peaks confirming the formation of silver nanoparticles in the composite while TGA indicated that silver nanoparticles contributed to good thermal stability of the composite. The formation of silver nanoparticles was indicated by a brown color transformation and an ultraviolet visible (UV Vis) absorption peak at 435 nm. The synthesized nanocomposite demonstrated promising antibacterial activity against both Staphylococcus saprophyticus DSM 18669 and Escherichia coli O157 strains, with S. saprophyticus showing higher susceptibility. This highlights the potential of chitosan-EDTA silver nanocomposites as alternative antimicrobial agents.

Industrial manufacturing method and characterization of Ayurvedic marine drugs: mother pearl, cowry, coral and pearl

Introduction: Ayurvedic marine drugs derived from mollusc shells and coral are regularly used by Ayurvedic physicians to treat several disease conditions like acid peptic disease, irritable bowel syndrome, osteoporosis, etc. However, standard operating procedures for manufacturing these drugs and their complete characterization have not been published in the Ayurvedic Formulary and Ayurvedic Pharmacopeia of India to date. Methods: Present study describes the traditional manufacturing process and thorough characterization using classical and advanced analytical tools. The raw materials characters, in-process parameters, and finished product specifications have been elaborated to develop monographs. Especially, the identity and purity of raw coral and pearl were checked by Raman Spectroscopy and Energy Dispersive X-ray Fluorescence analysis. Results: In the finished product analysis, the X-Ray Diffraction study revealed that incineration after trituration with Aloe barbadensis leaf pulp or rose water converted the aragonite phase of calcium carbonate into calcite phase in mother pearl, cowry, and pearl while the calcite form of raw coral was retained. The prominent bands around 1390, 870, and 712 cm−1 detected by Fourier Transform-Infrared Spectroscopy and mass loss between 39–44% (w/w) revealed by thermogravimetric analysis confirmed the carbonate form of these calcium-based drugs. The finished products were very fine grayish-white powders constituted by irregularly shaped nano-micro particulate calcium carbonate exhibiting particle size between 600 nm (D10 value) to 1.2 µm (D90 value). Conclusion: The quality control and assurance achieved in this study may be further utilized by the pharmaceutical industries to manufacture quality marine drugs and conduct efficacy studies.

Features of the iron determination in dust emissions of gas purification of electrometallurgical production

Features of the iron determination in dust emissions of gas purification at electrometallurgical facilities are considered. The elemental and phase compositions of dust emissions were determined using energy dispersive x-ray fluorescence analysis (EDXRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Sample preparation conditions were optimized with allowance for the analytical methods used. The phase composition of dust emissions represented mainly by zincite, zinc ferrite, halite and sylvite was preliminary determined by X-ray phase analysis. Model mixtures were prepared and used to construct calibration dependences taking into account the results of diffractometric studies. A technique for rapid x-ray fluorescence determination of iron in dust emissions of gas purification has been developed. The methods for iron determination tested on real samples of dust emissions of electrometallurgical production demonstrated a satisfactory convergence of the results obtained by EDXRF (Sr = 1.3%) and ICP-AES (Sr = 2.6%).

Investigation of the X‐ray fluorescence technique in the characterization of Ni coatings applied to historical heritage studies

AbstractHistorical heritage pieces allow a better comprehension of the characteristics of different civilizations over time. The characterization of such pieces is of paramount importance for their preservation. Energy‐dispersive X‐ray fluorescence (EDXRF) is recommended for this application, mostly because it is non‐destructive and the equipment is portable. However, one of its limitations is the difficulty in separating the signal from the substrate and the coating of multilayered samples, as it does not provide depth resolution. This project investigates the application of EDXRF in the characterization of metallic coatings, in the context of historical heritage. The elemental concentration of electrodeposited Ni coatings onto carbon steel substrates was obtained from EDXRF analyses. The relationship between the layer thickness and the variation of the Kα/Kβ intensity ratio of nickel peaks was exploited and the thicknesses of the coatings were estimated through EDXRF measurements. For comparison, particle‐induced x‐ray emission spectroscopy and scanning electron microscopy of the cross‐section were employed, providing a depth profile of the coatings. The estimated thicknesses from EDXRF analysis were comparable to those observed in the microscopy images for thinner films (up to 8 μm). On the other hand, for thicker films, the thicknesses were underestimated, due to the technique's depth limit and matrix effects, as secondary absorption. Despite these limitations, EDXRF remains valuable for evaluating cultural heritage pieces, often providing sufficient information to address authenticity concerns or to guide restoration processes. A case study was also performed to apply the methodology discussed on historical metallic pieces.

Influence of trace elements changes in the cerebellum on the rat’s behavior in elevated plus maze in the early period of mild blast-induced traumatic brain injury

The aim of the current study was to determine whether there are changes in brain trace elements of rats with blast-induced trauma and if these changes affect behavior in the elevated plus maze. Materials and methods. The study was carried out on 126 sexually mature male Wistar and were divided into 3 groups: Experimental – exposed to a shock wave 26.4 ± 3.6 kPa (n = 42); Sham (n = 42), the animals of which were subjected to inhalation anesthesia with halothane and fixation in a horizontal position; and Intact (n = 42). Behavior was study in elevated plus maze. The duration of presence in the open and closed arms, the number of stands, the duration of grooming was recorded in all groups of rats for 3 minutes. After, the animals were euthanized with halothane, followed by removal of the brain. The cerebellum was completely separated for spectral analysis using energy dispersive X-ray fluorescence analysis (EDRFA) on the analyzer EXPERT 3 XL. Results. Results showed significant changes of cognitive activity in experimental group which are indicate functional disorders of the cerebellum in the form of maladaptation in space with subsequent inhibition of motor centers. Cu/Fe ratio was decreased in the 14th and 21st days and increased in the 28th. Cu/Zn ratio was decreased on the 14th day. Zn/Fe ratio was higher on the 14th and 28th days. The existence of correlations between changes in trace elements and behavioral disorders in experimental rats was established. Conclusions. In the early period of blast-induced traumatic brain injury, cerebellar dysfunction in the form of spatial maladaptation with subsequent depression of motor centers was observed in the experimental rats Correlation analysis showed the presence of different strengths and directions of relationships between the ratios of Cu/Fe, Cu/Zn and Zn/Fe in the cerebellum and behavioral indicators in the elevated plus maze (duration of stay in open and closed arms, grooming and vertical motor activity) of experimental rats.

Possibilities of various arrangements of X-ray fluorescence analysis in the study of paintings

Energy dispersive X-ray fluorescence analysis (EDXRF) is a very useful method of elemental analysis in the study of works of art and archaeological finds, allowing the simultaneous non-destructive identification of a number of elements. A certain problem, if samples are not to be extracted from the investigated artifact, is its small depth range. However, this is not a serious drawback when it comes to the analysis of thin layers, such as plating or painting.In our laboratory, XRF was gradually developed and the equipment improved, with one of the main goals being the study of archaeological finds and works of art for the purposes of learning about the cultural heritage and restoration works.The presented paper aims to compare the possibilities of different macro- and micro-XRF instrumental arrangements in the study of paintings, from fast orientational measurement with a compact hand-held device through 2D scanning with a collimated beam to 3D analysis with collimated X-ray optics. Attention is paid to both the advantages and limitations of individual arrangements. A small painting by A. Piepenhagen, a typical representative of 19th century romantic landscape painting, was chosen as the object on which the possibilities of individual XRF variants are demonstrated.

X-ray fluorescence analysis in the study of paintings – an overview

Energy dispersive X-ray fluorescence analysis (EDXRF) is an excellent method in investigations of cultural heritage treasures, including easel and wall paintings and illuminations in ancient manuscripts. As one of the few methods applicable for this purpose, it is non-destructive and non-invasive. It is often combined with other methods such as optical microscopy, visible light photography, UV fluorescence photography, infrared reflectography, Fourier transform infrared spectroscopy, X-ray radiography, Raman spectrometry and others. The complex layered structure and mixtures of pigments, especially on easel paintings, represent a challenging task from the point of view of analysis. However, without taking samples it is only possible to analyse the thin surface layer of the investigated object with a thickness of tens to a few hundreds of micrometres. Nevertheless, this is not too much a problem when analysing paintings and even more so in the analysis of illuminations in manuscripts. The paper has an overview character and aims to summarise the possibilities, advantages and problems of XRF in this area and to demonstrate them on selected examples of published works, which in some cases are devoted to the works of leading painters from various historical periods (Giotto di Bondone, Antonello da Messina, Raffaelo Sanzio, Antonio Allegri da Corregio, Anthonis van Dyck, Rembrandt van Rijn, Giorgio Marini, Pablo Picasso and others). This review includes also a brief mention of selected research carried out in our laboratory.

Removal of Methylene Blue Dye in Aqueous System Using Polyvinyl Alcohol and Chemically Modified-Aluminium Foil Blend

Aqueous solution containing different concentrations of methylene blue dye was treated with chemically modified aluminium foil/PVA blends. There have been impressive decolourisation of the dye molecules in the aqueous system treated with the blends. Contact time and amount of composite facilitate more decolourisation of the dye solution. 97 % dye removal has been recorded at optimum conditions of the experiment. Energy dispersive X-ray fluorescence (EDXRF) analysis was used to determine the elemental composition of the aluminium foil and FTIR analysis was used to ascertain the composite formation between the foil and PVA. The blends have shown an impressive swelling property in aqueous system and poor to moderate in other organic solvents.

Inhibitory effect of UV and gamma radiation for fungal biodeterioration of concrete: A short-term study for sustainable conservation

The conservation of concrete-based deteriorated heritage buildings is a big challenging issue worldwide including in India. This study focused on to prevent fungal biodeterioration in concrete using UVC and gamma radiation. M20 graded concrete cubes (5 cm × 5 cm × 5 cm) were infected with Aspergillus tamarii, which was isolated from a 200 years old historic heritage building. M20 signifies a mixture of cement, sand and aggregate (1:1.5:3), made in such a way that the concrete cube has a compressive strength of 20 N/mm2 when examined after 28 days of curing. The fungal growth appeared clearly as calcium oxalate crystals in the Scanning Electron Microscope (SEM) photographs. Several doses of UVC and gamma radiation were applied on concrete cube. The changes in concrete properties were examined after 30 days in terms of weight, compressive strength, Fourier Transform Infrared Spectroscopy (FTIR) and micro Energy Dispersive X-ray Fluorescence (EDXRF). The results exhibited that compressive strength of control (non-infected and non-irradiated), biodeteriorated (infected), UVC (625 µw/cm² × 300 s) and gamma (0.5 KGy) irradiated infected (inhibition) concrete cubes were 19.74 ± 0.46, 18.88 ± 0.43, 20.20 ± 0.34 and 19.93 ± 0.20 N/mm2 respectively whereas negligible weight losses were observed for inhibition cubes compared to biodeteriorated ones. Calcite (1400, 874 and 705 cm−1), one of the major functional band present in concrete became weak after getting infected by Aspergillus tamarii and strong for inhibition samples irradiated with the above doses. The EDXRF analysis exhibited that mass percentage of calcium ions of the biodeteriorated concrete cubes (49.88 ± 0.65%) was lower than that of UV (75.75 ± 0.16%) and gamma (70.95 ± 0.30%) irradiated infected or inhibition concrete cubes. Altogether, the efficacy of the recommended inhibitory dose of ultraviolet and gamma radiation against concrete deterioration in the field of conservation of heritage building was observed to be positive.

CoPMoV Sulfide Catalysts Supported on Natural Halloysite Nanotubes in Hydrotreating of Dibenzothiophene and Naphthalene

Mixed sulfided CoMo catalysts supported on γ-Al2O3 and halloysite nanotubes (HNTs) were synthesized by incipient wetness impregnation with salt solutions of Keggin-type phosphorus- and vanadium-containing heteropolyacids. The synthesized materials were characterized by low-temperature nitrogen adsorption, energy dispersive X-ray fluorescence analysis, temperature-programmed reduction (both for the oxide and sulfide catalysts), and Raman spectroscopy, and were tested in hydrogenation of naphthalene and hydrodesulfurization of dibenzothiophene. The HNT-supported catalyst exhibited a greater activity in these reactions.

An augmented approach for the determination of the particle size effect on energy dispersive X-ray fluorescence analysis outcomes for alumina-based refractory materials

The chemical compositions of refractory materials, such as high-alumina concrete, bricks, and putty, were analyzed using an energy-dispersive X-ray spectrometer (EDXRF). An improved methodology for investigating the effect of particle size on the outcomes of EDXRF chemical analysis is presented. Eight independent refractory samples (refractory concrete, brick, and putty) were pulverized utilizing seven milling times (30, 60, 120, 180, 240, 300, and 360 s) and compared to non-pulverized samples. Thus, sixty-four refractory samples were obtained and analyzed using EDXRF. The method for measuring the fundamental EDXRF characteristics was then tested with ten certified reference materials. The acquired data were compared using inductively coupled plasma atomic emission spectrometry (ICP-OES). Univariate and multivariate statistics are used to evaluate EDXRF data. The particle size of the tested samples affected the z-scores of SiO2, Al2O3, Fe2O3, TiO2, CaO, MgO, Na2O, K2O, and P2O5 concentration measurements. Grinding times for refractory concrete, brick, and putty samples were determined in order to validate the robustness of the EDXRF technique and provide reliable chemical analyses. The ideal milling times for the samples studied ranged from 180 to 360 s, depending on the type of refractory material.

Use of elemental profiles determined by energy-dispersive X-ray fluorescence and multivariate analyses to detect adulteration in Ceylon cinnamon.

The price of Cinnamomum verum (Ceylon cinnamon) is around twice as high as that of the other cinnamon varieties commonly grouped under the name cassia cinnamon, making the former spice an attractive target for fraudsters. This work demonstrates that elemental profiles obtained by energy-dispersive X-ray fluorescence in combination with multivariate analyses can be used as a screening method to detect Ceylon cinnamon adulteration. Thirty-six elements were analysed in 52 commercially available cinnamon samples, 29 Ceylon, 8 cassia, and 15 for which no indication about variety was provided. Fifty-eight percent of the samples were either adulterated or did not meet international quality criteria. Four of the ground cinnamon samples labelled as Ceylon cinnamon were found to be pure cassia or a mixture with a high cassia content, and 26 samples were suspected of other types of adulteration including replacement of bark with other parts of the cinnamon tree. Headspace gas chromatography-mass spectrometry and ash determination by thermogravimetric analysis confirmed the conclusions reached by elemental analysis. Only one sample labelled as Ceylon cinnamon and that according to its volatile composition was cassia cinnamon was not flagged as suspicious by elemental analysis.

CoPMoV Sulfide Catalysts Supported on Natural Halloysite Nanotubes in Hydrotreating of Dibenzothiophene and Naphthalene

Mixed sulfided CoMo catalysts supported on γ-Al2O3 and halloysite nanotubes (HNTs) were synthesized by incipient wetness impregnation with salt solutions of Keggin-type phosphorus- and vanadium-containing heteropolyacids. The synthesized materials were characterized by low-temperature nitrogen adsorption, energy dispersive X-ray fluorescence analysis, temperature-programmed reduction (both for the oxide and sulfide catalysts), and Raman spectroscopy, and were tested in hydrogenation of naphthalene and hydrodesulfurization of dibenzothiophene. The HNT-supported catalyst exhibited a greater activity in these reactions.