Microanalytical characterization of decorations in handmade ancient floor tiles using inductively coupled plasma optical emission spectrometry (ICP-OES).

In this study a total of 114 glazed decorations of 42 ceramic floor tiles, manufactured in Sicily fromthe 16th to 19 the 21th AD, were investigated. The micro sampling method, proposed by us, using a cotton swab soaked in hydrofluoric acid, includes advantages of high sensitivity, high selectivity, simplicity, speed, not expensive and can be considered non-destructive because the point of sampling remains invisible to the human eye. ICP-OES technique was used in this study. Twenty-four elements (Al, As, B, Be, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Ni, Pb, Sb, Se, Si, Sn, Ti, V and Zn) were determined in each colored enamel. Enameled decorations in Sicilian tiles were varied in tones and chromatic effects, obtained with a limited 25 number compounds of cobalt, copper, iron, manganese, tin, and in the artifacts following the year 1920, also titanium. An important remark is that some of the colors, such as black, orange, purple and brown were prepared using the same metals, while white, light blue, blue and green were obtained with different elements. The adoption of different recipes for the same color suggests the presence of several laboratories of ceramists working in Sicily who had preferences for different methods for the production of their enameled artifacts. Concerning the opacifier, the high amounts of lead and antimony, only in a case, indicate the use of lead antimonate (Pb2Sb2O7). Black decorations were present in several of the analyzed samples and in most of them were identified mixtures of black iron and manganese oxides. The green decorations appear to have been prepared with copper oxide; lighter hue samples contained additional amounts of zinc and/ or barium compounds. Considering all the samples, meanly, iron predominates in yellow decorations, only a sample contains large amounts of Cd, Zn and very little Sb, which suggests the use of the pigments ZnO as white) and CdS as cadmium yellow. For all samples, except one, we can exclude the use of pigments containing chromium

The PAH composition in limpets (Patella vulgate L.) from the coasts of Sicily (Italy)

This article examines the presence, distribution, nature and sources of 19 Polycyclic Aromatic Hydrocarbons (PAH), in Patellae (patella vulgate L.) and seaweed (vulva) sampled in different stations of Sicilian coastal environments and analyzed for their polycyclic aromatic hydrocarbon (PAH) content. Analysis was performed by gas chromatography/mass spectrometry (GC/MS) with selected ion monitoring (SIM), after saponification of the sample and clean up of the extract. In the limpets the total concentration of polycyclic aromatic hydrocarbons ranged from 34 to 750 μg/Kg of dry matrix. The relative standard deviation (RSD) of the replicas on the concentrations of individual compounds ranged from 4 to 20%. The accuracy of method was estimated by analyzing "blank" samples spiked with known quantities of analytes and the recover percentage was 82 ± 12%. The detection limit (LOD) of analytical procedure was less than 0.2 μg/Kg d.w. for all analytes. The quantification limit (LOQ) of analytical procedure was less 0.7 μg/Kg d.w. The resulting distributions and weight ratios of specific compounds are discussed in terms of sampling location and origin. The results obtained show that levels of contamination vary from one sampling station to the next, while relative distributions of PAH is homogeneous in most stations. Lipidic content and total PAH concentrations were found not to be correlated and the compounds present in limpets were shown to be mainly of petrogenic origin. There is no evidence of coal-tar contamination. Copyright © 2006 Taylor & Francis Group, LLC

Quantification of Platinum in Edible Mushrooms Using Voltammetric Techniques

Edible mushrooms are a food source with interesting nutritional values. The chief objective of this research was to develop a consistent method for the quantitative ultra-trace analysis of Pt in mushrooms, which is complex because it cannot be readily quantified by common analytical procedures. This research is one of the first analytical methods to establish Pt amount in these vegetables. In this research, 28 different edible mushroom samples from Italy were investigated. Determination of Pt in mushrooms was completed using Differential Pulse Voltammetry (DPV). In this study, we applied the standard addition method because there are no certified reference mushrooms containing platinum group elements on the market. The platinum quantification limit was 0.03 µg kg−1 d.w. In the analyzed samples, platinum amount was in the range of 0.03–73 µg kg−1 . Our mushroom samples had a Pt content lower than the concentrations recommended by international establishments for other foodstuffs. In the future, the optimized method could be used for the analysis of plant and animal matrices intended for food supply

Photochemical sample treatment for extracts clean up in PCB analysis from sediments

Sample purification can be considered the most polluting step of the whole analytical process for PCBs determination in sediment samples. The use of photochemical sample treatment represents an alternative methodology for extracts clean up allowing for a reduction of the used amount of organic solvents. The first application of a photochemical sample treatment for the selective removal or reduction of organic substances interfering with PCBs analyses in sediments is reported. The method's efficiency and robustness were compared with currently used chromatographic purification. Quality parameters such as recovery, linearity and reproducibility were studied. The entire procedure was validated by four replicate analysis of certified reference sediment. The quantification limits (LOQ) obtained by us ranged from 1 to 3.1 ng g(-1). The RSD for each congener was below 15\% and recoveries were in the range 40-130\%. Results based on the analysis of real and certified samples showed similar or improved detection thresholds and pointed out the advantages of the photochemical methodology in terms of costs and environmental friendly conditions. (C) 2012 Elsevier B.V. All rights reserved

The effect of montmorillonite clay in alginate gel beads for polychlorinated biphenyl adsorption: Isothermal and kinetic studies

Beads of alginate montmorillonite have been used as sorbent for polychlorinated biphenyls from aqueous solutions.The structure and the differences between the different beads were established by IR spectroscopy (FT-IR). The adsorption at 25 °C has been studied in a batch system, following its kinetics and assessing adsorbent dose, initial PCB concentrations, and pH effects. The results show that increasing the initial concentration of the PCBs and the adsorption time favored the adsorption. Adsorption isotherm data were modeled using Chapman, Freundlich and Langmuir adsorption isotherms and the appropriate parameters were calculated.Adsorption of trichlorobiphenyls on alginate–montmorillonite beads followed a Freundlich isotherm type model, while adsorption of tetra-, penta-, and hexachlorobiphenyls displayed a sigmoid-shaped (S-type) isotherm fitting the Chapman sigmoidal equation with the highest non-linear R2 values among the three tested models. By comparing the percentage adsorptions using the same number of beads (same volumes), best removals were obtained by using alginate montmorillonite beads.Adsorption of trichlorobiphenyls on alginate–montmorillonite beads followed a Freundlich isotherm type model, while adsorption of tetra-, penta-, and hexachlorobiphenyls displayed a sigmoid-shaped (S-type) isotherm fitting the Chapman sigmoidal equation with the highest non-linear R2 values among the three tested models. By comparing the percentage adsorptions using the same number of beads (same volumes), best removals were obtained by using alginate montmorillonite beads.Adsorption of trichlorobiphenyls on alginate–montmorillonite beads followed a Freundlich isotherm type model, while adsorption of tetra-, penta-, and hexachlorobiphenyls displayed a sigmoid-shaped (S-type) isotherm fitting the Chapman sigmoidal equation with the highest non-linear R2 values among the three tested models. By comparing the percentage adsorptions using the same number of beads (same volumes), best removals were obtained by using alginate montmorillonite beads.Adsorption of trichlorobiphenyls on alginate–montmorillonite beads followed a Freundlich isotherm type model, while adsorption of tetra-, penta-, and hexachlorobiphenyls displayed a sigmoid-shaped (S-type) isotherm fitting the Chapman sigmoidal equation with the highest non-linear R2 values among the three tested models. By comparing the percentage adsorptions using the same number of beads (same volumes), best removals were obtained by using alginate montmorillonite beads. Kinetic models were investigated to determine the mechanism of adsorption showing a best fit for the pseudo second order model (R2 from 0.998 to 0.982. Moreover, to underline the effect of montmorillonite in alginate gel beads, we have compared the isothermal adsorption curves between alginate montmorillonite and alginate beads

Macro and micro elements in traditional meals of Mediterranean diet: Determination, estimated intake by population, risk assessment and chemometric analysis

The aim of the study was to estimate the dietary exposure of the main macro and micro elements from meals typically consumed by the Mediterranean population, in particular Sicilian by samples prepared and cooked prior to analysis. A total of 57 typical Mediterranean meals samples were analysed for 4 macro elements: Calcium (Ca), Potassium (K), Magnesium (Mg) and Sodium (Na) and 13 micro elements: Aluminium (Al), Arsenic (As), Cadmium (Cd), Cobalt (Co), Chromium (Cr), Copper (Cu), Iron (Fe), Mercury (Hg), Manganese (Mn), Nickel (Ni), Lead (Pb), Zinc (Zn) and Vanadium (V) by inductively coupled plasma - mass spectrometry and atomic absorption spectrometry. Mercury concentration was quantified directly on the food samples by using the DMA-80 (Direct for Mercury Analysis). Daily Estimated Element Intake was calculated for essential element and assessment of health risk associated with intake of investigated elements was performed. In particular, analysed samples supply from 3.7% to 62% of sodium, 0.05–19% of potassium, 0.1–3.2% of calcium, 1.6–16% of magnesium, 2.1–37% of iron, 0.7–48% of zinc and 0.98–339% of chromium. some of the foods prepared are lacking in all macroelements (Na, K, Ca, Mg). The quantity of macroelements taken from a single portion of 100 g of several food, compared to the recommended quantities, is low, but it should be considered that on average in one day (breakfast, lunch and dinner), undoubtedly, the inhabitants of the Mediterranean area consume much higher quantities for a total of 500–1000 g, therefore, this study confirmation for the populations concerned, the low probability of nutritional or health risks due to the consumption of foods, indeed, the consumption of Mediterranean dietary foods, has not shown particular risk assessments from heavy metals

Matrix-matched quantification of volatile organic compounds (VOCs) in gluten free flours and bakery products

The aim of this study deals with characterize the volatile profiles of gluten free flours and bakery products. An appropriate HS-SPME/GC-MS methods for the quantification analyses was performed and corn starch solid as standards was used. 34 different samples were analysed, and 127 compounds distributed in 4 classes (alcohols, aldehydes and ketones, heterocyclic compounds, and terpenes), that make up the aroma of these gluten free, were identified. The developed method is characterized by detection limits of 0.0004 and 0.0047 mg/kg for camphor and pyrazine, respectively, and linearity of quantification standards were between 0.990 and 0.998 for a range of 3-50 mg/kg

Polycyclic Aromatic Hydrocarbons (PAH) in Volcano island (Aeolian archipelago) mud utilized for therapeutic purpose

This paper examines the possible presence, distribution, nature and sources of 18 Polycyclic Aromatic Hydrocarbons (PAHs) as constituent of the muds pool collected in Vulcano Aeolian Island. PAHs are important from environmental and toxicological point of view. Analysis was performed by gas chromatography/mass spectrometry (GC/MS) in selected ion monitoring (SIM). The total concentration of Polycyclic Aromatic Hydrocarbons ranged from 112 to 154 g/Kg of dry matrix. The volcanic muds, used for therapeutic purposes, are moderately contaminated

Occurrence and concentration of PAHs in clams and sediments of the marine coastal lagoon of Ganzirri (Italy). Extraction, GC-MS analysis, distribution and sources

The distribution of selected Polycyclic Aromatic Hydrocarbons (PAHs) in surface sediments and clams of marine coastal lagoons, called Ganzirri, located at the Sicilian coast of the, Messina's strait, has been investigated by GC/MS analysis with Selected Ion Monitoring (SIM) mode. The lagoon is characterized by abundant organic detritus, deriving from aquagenic and anthropogenic inputs. Anoxic/reduced conditions of sediments make them a preferential site for uptake and preservation of PAHs. From an eco-toxicological point of view, the aquatic ecosystem investigated appears to be moderately polluted. The investigations have been performed on the 16 PAHs recommended by US-EPA as priority pollutants to be monitored in the framework of environmental quality control. The sediment PAH concentrations ranged from 135 to 1650 mu g/kg dry matrix. The total concentrations of PAHs in clams ranged from 60 to 1427 mu g/kg d.w. The relative standard deviation (RSD) for all samples of the concentration replicates of individual compounds ranged from 10% to 25%. The resulting distributions and ratios of specific compounds have been discussed in terms of sampling location and origin of contaminants. The results obtained show that levels of contamination are not homogeneous throughout the stations. In the Ganzirri Lagoon, the bioavailability of hydrophobic organic compounds, such as PAHs, seems to be mainly governed by chemical characteristics of the contaminants. Pyrolytic compounds (penta- and hexa-aromatics) are not readily available. In contrast, petroleum hydrocarbons (some tetra-aromatics) are accumulated by clams to a great extent