Direct multielement determination of trace elements in boron carbide powders by direct current arc atomic emission spectrometry using a CCD spectrometer

The use of direct current arc atomic emission spectrometry (DC-arc-AES) with a CCD spectrometer for the direct determination of the trace impurities Al, Ca, Cr, Cu, Fe, Mg, Mn, Na, Ni, Si, Ti, and Zr in three well characterized boron carbide powders is described. The detection limits obtained by the procedure were found to be between 0.2 (Mg) and 25 (Na) ??g?g^?1 for the above elements. Three boron carbide powder samples with trace element concentrations between 0.9 (Cu) and 934 (Si) ??g?g^?1 for Al, Ca, Cr, Cu, Fe, Mg, Mn, Na, Ni, Si, Ti, and Zr ?? including the standard reference material ERM?-ED102 ?? were analyzed by DC-arc-AES. The relative standard deviations for 9 measurements when using 5.0?±?0.3?mg of the respective samples were found to vary from 6.2 to 27% for Al and Cu, respectively. The trace elements Al, Ca, Cr, Cu, Fe, Mn, Ni, Si, Ti and Zr could be determined in the standard reference material and their concentrations determined by DC-arc AES were found to be between 89 and 116% of the accepted values. Fe and Ti were determined by DC-arc AES in the three boron carbide samples as well as in Al₂O₃, BN, SiC, coal fly ash, graphite and obsidian rock. The correlation coefficients of the plots of the net intensities versus the accepted values over the concentration ranges from 18 to 1750 and from 6 to 8000???g?g^?1 are 0.999 and 0.990 for Fe and Ti, respectively.

Determination of Trace Elements in Dendrobium Officinale Cultivated in Various Conditions

Dendrobium officinale is an important medicinal plant in traditional Chinese medicine. The consumption of D. officinale has increased rapidly in recent years due to the health awareness among Chinese people. The present study aimed to determine trace elements levels in 42 D. officinale samples and to utilize the elemental data for identifying the cultivation technique. Eighteen trace elements (B, V, Cr, As, Mn, Fe, Mo, Cu, Zn, Se, Sr, Sn, Ti, Al, Co, As Pb, Cd, and Bi) were determined by inductively coupled plasma–mass spectrometry. Of the 11 essential elements, the mean concentrations ranged from 30.6?µg?kg^?1 (Mo) in D. officinale with greenhouse cultivation to 161?mg?kg^?1 (Fe) in D. officinale with rock cultivation, and the contributions of Mn may exceed the dietary reference intake value by the uptake of 20?g of D. officinale. Of the seven toxic elements, the mean concentrations ranged from 3.29?µg?kg^?1 (Bi) in the D. officinale with greenhouse cultivation to 342?mg?kg^?1 (Al) in the D. officinale with rock cultivation, and the contributions of Al may exceed the provisional tolerable daily intake value by the uptake of 20?g of D. officinale. The concentrations of seven metals (Bi, Pb, Fe, Al, Cr, As, and Mo) were utilized to identify the cultivation technique of the analyzed D. officinale samples through linear discriminant analysis.     

Application of nondestructive X-ray fluorescence analysis to determine the element composition of medicinal plants

A nondestructive X-ray fluorescence technique has been developed to determine Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr, Ba, and Pb in plants. The line element intensities were measured by an S4 Pioneer X-ray sequence spectrometer (Bruker AXS, Germany). The inversely proportional relationship was obtained between the analyte line intensity and mass of the plant, pressed on boric acid backing, for elements with an atomic number 11 < Z < 20. It was found that reduction of plant mass from 6 to 1 g leads to an increase in element determination sensitivity. The detection limits for 1 g of pressed plant were evaluated as μg/g: 5–20 (Na, Mg, Al); 1–4 (Si, P, S, Cl, K, Ca, Ti, Ba, Pb); 0.4-0.8 (Cr, Mn, Fe, Ni, Br, Cu, Zn, Rb and Sr). This technique was applied to determine the element composition of violets of Violaceae family, which are used in medicine.     

A new approach for determination of crustal and trace elements in airborne particulate matter

An ICP-OES procedure was developed for fast and accurate determination of various crustal (Al, Ca, Fe, Mg, Si) and trace elements (Ba, Cu, Mn, Na, K, Sr, Ti, Zn) in airborne particulate matter. The method is based on a preliminary treatment of the aerosol samples with a mixture of nitric acid and hydrogen peroxide at elevated temperature leading to a mineralization of the organic sampling substrate, dissolution of soluble material and homogeneous suspension of the remaining non-soluble fraction. After dilution the derived slurry solutions were measured using ICP-OES. The reproducibility of analysis given as the relative standard deviation (% RSD) varied between 3.2 and 6.8% for bulk constituents such as Al, Ca, Fe, Mg and Si whereas values ranging from 3.5 to 9.1% were obtained for trace metals present with distinctly lower abundance in PM10 (e.g. Ba, Cu, Mn, Sr, Zn). The limits of detection (LOD) calculated as three times the standard deviation (3σ) of the signal derived from filter blank samples ranged from approximately 1?ng?m^?3 (Sr) to 71?ng?m^?3(Ca). The developed procedure was evaluated by comparing the obtained results with the findings derived for the same set of aerosol samples analyzed using a microwave procedure for sample dissolution with subsequent ICP-OES analysis. Finally the developed procedure was applied for the analysis of crustal and trace elements in PM10 samples collected at an urban site (Getreidemarkt, Vienna) and a rural site (Hartberg, Styria), in Austria. The concentrations of the investigated crustal elements varied between some hundred ng?m^?3 and few µg?m^?3 with highest concentrations for Fe and Si, distinctly reduced concentrations ranging from some ng?m^?3 (Sr) to more than hundred ng?m^?3 (K) were found for trace elements. Observed PM10 concentrations were found to be in accordance to literature findings from urban sites in central Europe.     

Strontium and cesium sorption of some Anatolian zeolites

Zeolite samples of Tertiary age obtained from different areas of Anatolia (Turkey) are classified as Clinoptilolite, Analcime or Heulandite and we have investigated their sorption capacity for Cs⁺ and Sr²⁺ ions from aqueous solutions. Quantitative analysis of the zeolite samples untreated and treated with chloride salts of Cs⁺ or Sr²⁺ in aqueous solutions, for Na, Mg, Al, Si, P, K, Ca, Ti, Mn and Fe were performed using EDXRF. Chemical analysis indicated that the Clinoptilolite type zeolite from the deposits of Cankiri-Corum Basin of Anatolia is the best sorber for Sr and Cs ions.Presented at the Sixth International Seminar on Inclusion Compounds, Istanbul, Turkey, 27–31 August, 1995.     

Investigation of the interaction of Greek dolomitic marble with metal aqueous solutions using rutherford backscattering and X-ray photoelectron spectroscopy

To enhance the applicability of the nuclear analytical technique in the field of industry and the environment, the inorganic elemental content of the bottom ash from a municipal solid waste incinerator was determined by instrumental neutron activation analysis. Bottom ash samples were monthly collected from an incinerator located at a metropolitan city in Korea, strained through a 5 mm sieve, dried by an oven and pulverized by an agate mortar. The samples were irradiated at the NAA #1 irradiation hole (thermal neutron flux: 2.92·10¹³ n·cm⁻²·s⁻¹) in the HANARO research reactor of the Korea Atomic Energy Research Institute and the irradiated samples were measured by a HP Ge gamma-ray spectrometer. Thirty-three elements including As, Cr, Cu, Fe, Mn, Sb and Zn were analyzed by an absolute method. The quality control was conducted by a simultaneous analysis with NIST standard reference materials. The average concentrations of the major elements such as Ca, Fe, Al, Na, Mg, K and Ti measured in the sample were 19.9%, 4.85%, 3.79%, 2.11%, 1.84%, 1.22% and 1.02%, respectively. In addition, the concentrations of the hazardous metals like Zn, Cu, Cr, Sb and As were 0.77%, 0.31%, 729 mg·kg⁻¹, 116 mg·kg⁻¹ and 22.2 mg·kg⁻¹, respectively.     

Geochemistry study of soil affected catastrophically by tsunami disaster triggered by 2004 Indian Ocean earthquake using a fourth harmonics (λ = 266 nm) Nd:YAG laser induced breakdown spectroscopy

In this work, laser induced breakdown spectroscopy (LIBS) analysis of the soil samples collected from Aceh, a place in Indonesia worst affected by 2004 Indian Ocean tsunami, was conducted. In the LIBS experimental system, a high energy pulsed laser beam was focused on the tsunami affected soil samples and the atomic emission lines, originating from the laser induced plasma were recorded using locally developed laser induced breakdown spectrometer. Our results show that the concentrations of many elements especially terrestrial markers, namely titanium, iron, and carbonate marker such as magnesium, are higher in the tsunami-affected samples than that in the unaffected samples collected from the same neighborhood. The quantification of Ti, Fe and Mg were carried out using Ti II 334.94, Fe I 438.35, and Mg I 277.98 nm atomic transition lines respectively by drawing the calibration curve by preparing the samples of known concentrations in unaffected soil matrix. In order to ensure accurate quantification, the local thermal equilibrium of the laser-induced plasma was verified using Mc Writher criterion, for which the plasma temperature was estimated using linearized Boltzmann plot for six iron atomic transition lines and the electron number density in the plasma was estimated using Stark broadened Fe I 540.4 nm atomic lines. The estimated temperature and electron number density of the laser induced plasma are 9642 K and 3.5 × 10¹⁶ cm^?3 respectively. The concentrations of Ti, Fe and Mg in tsunami unaffected soil are 0.09, 3.2 and 0.02 w/w% and in tsunami affected soil are 0.14, 7.9 and 0.048 w/w% respectively. These values are in good agreement with XRF data. The elemental ratios extracted from LIBS signal intensity revealed that LIBS emission intensity ratios of several elements, such as Si/Ti, Al/Ti and Sr/Ba are potential candidates as the distinctive geochemical signature for identification the soil impacted and unimpacted by the 2004 Indian Ocean giant tsunami. The advantage of using LIBS for the elemental analysis is that the sample can be analyzed in its pristine form without any need cumbersome sample preparation method, which has the risk of bringing in external additives through chemicals used for the sample preparation. Other advantages of LIBS technique are that the analysis can be in situ and can be carried out remotely.     

Experimental assessment of a large sample cell for laser ablation-ICP-MS, and its application to sediment core micro-analysis

The coupling of laser ablation (LA) to inductively coupled plasma-mass spectrometry (ICP-MS) enables the direct analysis of solid samples with micrometric resolution. Analysis is often restricted to relatively small samples owing to the dimensions of conventional ablation cells. Here, we assess the performance of a large rectangular, commercially-available sample cell which enables analysis over a 10.2?×?5.2 cm² area. Comparison with the conventional cell shows a small to moderate performance decrease for the large cell resulting from the dilution of ablated particles in a larger volume with a 4–31% lower signal output and longer signal tailings. The performance of this cell is however sufficient for the determination of both major and trace elements in many kinds of samples. The applicability of the large cell LA-ICP-MS setup was demonstrated by the determination of Al, Si, Mn, Fe, Cu, Zn Pb and U in sediment core sections at a resolution of 0.6 mm. Detection limits for sediment analysis were 7 mg Al kg^?1, 68 mg Si kg^?1, 0.5 mg Mn kg^?1, 20 mg Fe kg^?1, 0.2 mg Cu kg^?1, 0.3 mg Zn kg^?1, 0.08 mg Pb kg^?1 and 0.003 mg U kg^?1. Cyclic patterns, which would have been overlooked by conventional analysis at cm resolution, were observed in analysed sediments. This study demonstrates the potential of LA-ICP-MS in environmental analysis, with the large sample cell setup offering the possibility to analyse a wider range of samples without sectioning.     

Retrospective determination of 238Pu, 239,240Pu and 90Sr activities in the outer bark of Norway spruce (Picea abies (L.) Karst.) collected at various sites in the Czech Republic

The activity concentrations of ²³⁸Pu, ^239,240Pu and ⁹⁰Sr were determined in 25 archived spruce outer bark samples collected in coniferous forests across the Czech Republic in 1995. At three sampling sites the radionuclide activity concentrations were determined in forest soil. Data was provided on the cumulative deposition and vertical distribution of ²³⁸Pu, ^239,240Pu and ⁹⁰Sr in forest soil. The median activity concentration of ²³⁸Pu in the spruce bark samples was 0.009 Bq kg^?1. The median activity concentration of ^239,240Pu was 0.212 Bq kg^?1, and the median activity concentration of ⁹⁰Sr was 10.6 Bq kg^?1. The radionuclide activity concentration distribution was not significantly explained by the local long-term (1961–2000) mean annual precipitation totals, by site elevation, by bark acidity, by soil moisture and soil texture. The activity concentrations of the radionuclides in bark were found to be higher than or comparable with the published and measured figures for radionuclide activity concentrations in cultivated and uncultivated soils (0–20 cm layer) in the Czech Republic and abroad. The activity concentration ratio of ⁹⁰Sr/^239,240Pu in the investigated spruce bark samples was higher than in the relevant soil samples. We assume that the crucial radioactive contamination loads in bark occurred in the first half of the 1960s, when the concentration of the investigated radionuclides in the air was highest. Spruce trunk bark has preserved relatively high activity concentrations of these radionuclides. The mechanism governing the long-term radionuclide activity concentrations in outer bark proportional to the local radioactive fallout rates is not correctly known. Our results indicate the suitability of spruce bark for use as an effective monitor of radioactive plume fallout loads even several decades after the contamination episode.     

Verfahren zur Spurenanalyse aus metallischen Proben

Zusammenfassung Ein neues lösungsspektrographisches Zerstäubungsverfahren wird beschrieben, bei dem die Lösung so zerstäubt wird, daß sie die Graphitelektroden nicht berührt. Mit diesem Verfahren könnten 10^–3 bis 10^–5 % Al, B, Cr, Cu, Mg, Mn, Mo, Ni, Si, Sn, Ti, V und Zr in Eisen und Stahl bestimmt werden.Zur Bestimmung von Verunreinigungen oder Einschlüssen in Stahl wird ein spektrographisches Verfahren mit Preßlingselektroden empfohlen, das nur 0,1–1 mg Rückstand benötigt. Oxide von Al, B, Ca, Co, Cu, Cr, Fe, Mg, Mn, Mo, Nb, Ni, Pb, Si, Sn, Sr, Ti, V, Zn und Zr konnten bis herab zu etwa 10^–7 g erfaßt werden.

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Methods for the determination of trace elements from metallic samples

The principles of a new spectrographical atomizing-method of solution are described. The solution has to be atomized into a gap without contacting the surface of the graphite electrodes. In this way the exact determination of 10^–3 to 10^–5 % of Al, B, Cr, Cu, Mg, Mn, Mo, Ni, Si, Sn, Ti, V and Zr in iron and steel is possible.The microanalytical determination of impurities or inclusions in steel has been achieved by a spectrographical method with briquette electrodes. The necessary amount of isolation residue is only 0.1–1 mg. The oxides of Al, B, Ca, Co, Cu, Cr, Fe, Mg, Mn, Mo, Nb, Ni, Pb, Si, Sn, Sr, Ti, V, Zn and Zr can be accurately determined by this procedure. The limit of determination is about 10^–7 g.

     

Major,trace, and natural radioactive elements in bituminous coal from Australia,Romania, Russia,South Africa and Ukraine: A comparative study

Summary Five samples of bituminous coal collected from different basins (Australia, Romania, Russia, South Africa and Ukraine) have been investigated by using different analytical techniques. Na, Mg, Al, Cl, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Rb, Sr, Mo, Sn, In, Sb, Cs, Ba, La, Ce, Nd, Sm, Eu, Gd, Tb, Dy, Lu, Hf, Ta, W, Hg, Th and U have been determined by neutron activation analysis, ⁴⁰K, ²³⁸U, ²³⁵U and ²³² Th have been measured radiometricaly, H, C, O, N, and S have been dosed by dynamic flash combustion, while gravimetric methods have been used to measure moisture and ash content together with calorific power. Major mineralogical fractions have been investigated by means of X-ray diffraction. The results have shown significant positive correlations between radiometric and activation analysis results, between calorific power and carbon, nitrogen and hydrogen concentrations and negative significant correlations between calorific power and ash content. According to the Romanian Regulations, only Cr and Ni for Romanian coal exceeded the minimum threshold to be considered unpolluting elements. The distribution of rare earth elements, La to Th ratio, as well as of Sc, La and Th together with Co, Hf and Th have confirmed that, irrespective of sample sources, the mineral part of coal has a composition close to that of the upper continental crust.     

燃煤飞灰中铁质微珠的显微结构及其组成研究

选用我国三个典型燃煤煤种的电厂飞灰中铁质微珠,进行显微结构与物相组成等方面的研究。揭示出铁质微珠中存在空心微珠、子母珠和实心微珠三种显微颗粒类型,在这些显微颗粒表面可识别出以微粒状和八面体自形晶两种方式存在的赤铁矿和磁铁矿析晶;元素分析表明,燃烧褐煤电厂铁质微珠主要由Fe、Ca、Al、和Si元素组成,燃烧烟煤和无烟煤的电厂铁质微珠主要由Fe、Al和Si元素组成;物相分析发现,Fe在铁质微珠中以四种存在形式：Fe3O4、α-Fe2O3、γ-Fe2O3和Fe3+-玻璃相。这些物相在三个电厂飞灰中呈现出不同的分布特征,反映出不同的燃煤煤种在锅炉中燃烧温度的差异。随着温度的升高,Fe3O4先氧化为γ-Fe2O3,或γ-Fe2O3与Fe3O4的固熔体,然后再转变为α-Fe2O3,当温度超过 1 400 ℃时,Fe2O3又转化为Fe3O4。     

Studies on adsorption and separation characteristics of americium and lanthanides using a silica-based macroporous bi(2-ethylhexyl) phosphoric acid (HDEHP) adsorbent

Activity concentrations of ⁹⁰Sr in samples of wild boar bones hunted in different regions of Slovakia were determined. Molecular recognition technology product IBC´s AnaLig^®Sr-01 and tributyl phosphate were used for strontium determination. From 7 to 10 g of bone ash was used for ⁹⁰Sr analysis. Both separation methods were statistical tested and compared. The presented results were evaluated as correct for all experimental data for ⁹⁰Sr determination in ash bone samples. Activity concentrations of ⁹⁰Sr in bones were in the range of (4.5–69.0) Bq kg^?1.     

Evaluation of strontium isotope abundance ratios in combination with multi-elemental analysis as a possible tool to study the geographical origin of ciders

In order to evaluate alternative analytical methodologies to study the geographical origin of ciders, both multi-elemental analysis and Sr isotope abundance ratios in combination with multivariate statistical analysis were estimated in 67 samples from England, Switzerland, France and two Spanish regions (Asturias and the Basque Country). A methodology for the precise and accurate determination of the ⁸⁷Sr/⁸⁶Sr isotope abundance ratio in ciders by multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) was developed. Major elements (Na, K, Ca and Mg) were measured by ICP-AES and minor and trace elements (Li, Be, B, Al, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Y, Mo, Cd, Sn, Sb, Cs, Ba, La, Ce, W, Tl, Pb, Bi, Th and U) were measured by ICP-MS using a collision cell instrument operated in multitune mode. An analysis of variance (ANOVA test) indicated that group means for B, Cr, Fe, Ni, Cu, Se, Cd, Cs, Ce, W, Pb, Bi and U did not show any significant differences at the 95% confidence level, so these elements were rejected for further statistical analysis. Another group of elements (Li, Be, Sc, Co, Ga, Y, Sn, Sb, La, Tl, Th) was removed from the data set because concentrations were close to the limits of detection for many samples. Therefore, the remaining elements (Na, Mg, Al, K, Ca, Ti, V, Mn, Zn, As, Rb, Sr, Mo, Ba) together with ⁸⁷Sr/⁸⁶Sr isotope abundance ratio were considered for principal component analysis (PCA) and linear discriminant analysis (LDA). Finally, LDA was able to classify correctly 100% of cider samples coming from different Spanish regions, France, England and Switzerland when considering Na, Mg, Al, K, Ca, Ti, V, Mn, Zn, As, Rb, Sr, Mo, Ba and ⁸⁷Sr/⁸⁶Sr isotope abundance ratio as original variables.     

Determination of metal impurities in ultrapure CaCl2 and MgCl2 by ICP OES

An effective, rapid and simple analytical method for the determination of Na, K, Ca, Mg, Cd, Pb, Ba, Fe, Mn, Sr, Zr, Cu, Zn and Al at mg kg⁻¹ levels in the ultrapure salts MgCl₂ and CaCl₂ using optical emission spectrometry was developed. Optimisation of the operation conditions was performed with real samples of ultrapure MgCl₂ and CaCl₂. The results of the determination with multi-elemental water standards were compared to the internal standardisation, the standard addition method, and the maximum allowable content of the above mentioned elements in pure chemicals. The method was shown to be very sensitive with the following limits of detection: Na 1.01, K 3.12, Ca 0.263, Mg 0.275, Cd 0.0832, Pb 0.482, Ba 0.0153, Fe 0.0528, Mn 0.0473, Sr 0.0203, Zr 0.638, Cu 0.0732, Zn 0.0686 and Al 0.459 (all in mg kg⁻¹). The method exhibited satisfactory precision, high analytical recoveries, linear responses of an accuracy of at least 4 orders of magnitude and low contamination susceptibility.     

Dry-Ashing Preconcentration for Micro-Reactor-Based Neutron Activation Analysis of Food and Plant Samples

The application of preconcentration by dry-ashing to the neutron activation analysis of biological samples using a SLOWPOKE-2 low-power reactor is reported. Samples of selected food crops (banana, callaloo, carrot, mango, and yam) and bioindicator plants (lichen, moss, Tillandsia sp., and tree bark) were analysed both as plant tissue, and as ashed sample. The results are presented for 21 elements. Good agreement between both procedures (<10% relative standard error) was obtained for 13 elements: Al, Ca, Cd, Cr, Fe, K, La, Mg, Mn, Na, Sm, Ti, and V. For Dy, Rb, and Zn the agreement was 10-15%. Relatively poorer agreement (>15-30%) was obtained for As, Br, Cl, and Sb. Dry ashing produced improved analytical results for those samples that were of low ash content. However, the increased background counts observed in ashed samples can sometimes negate the concentration gain, particularly in plants with high ash contents but low levels of certain elements.     

Determination of trace elements of some Egyptian crops by instrumental neutron activation,inductively coupled plasma-atomic emission spectrometric and flameless atomic absorption spectrophotometric analysis

Instrumental neutron activation analysis was used for the determination of Al, Br, Ca, Ce, Cl, Co, Cr, Cs, Eu, Fe, K, La, Mg, Mn, Na, Rb, Sb, Sc, Se, Ti, Th, V and Zn, ICP-AES for the determination Al, Ag, Ba, Be, Ca, Co, Cr, Cu, Fe, Ga, K, Li, Mg, Mn, Na, Ni, P, Sc, Sr, Ti, V and Zn and flameless AAS for the determination of Cd, Hg and Pb in egg plant, potatoes, green pepper (Leguminosae), vegetable marrow (Cucurbitaceae), pears, apple (Rosaceae), castor oil plant (Euphorbiaceae), lettuce (compositae), dill, parsley, coriander (Umbelliferae), and in some soil samples collected from Aswan province.     

Radioanalytical methods for the non-destructive analysis of lunar samples

The elemental compositions of Apollo 11 and Apollo 12 lunar soil samples 10084,141 and 12070,83 and Apollo 12 rock fragment 12063,73 were determined by non-destructive radioanalytical methods. Main mineral fractions and glasses separated from these samples were analyzed as well. Instrumental neutron activation analysis (INAA) was used to determine Na, Mg, Al, Si, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Zr, Cs, Ba La, Ce, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Tm, Yb, Lu, Hf, Ta, W, Ir, Au, Th and U. A method of delayed neutron counting was used for the determination of uranium, and non-dispersive radioisotopic X-ray fluorescence analysis was applied to the determination of Ti, Fe, Sr, Y and Zr.     

Chemical characterization of ancient potteries from Himera and Pestavecchia necropolis (Sicily, Italy) by Inductively Coupled Plasma–Optical Emission Spectrometry (ICP–OES)

Thirty-eight samples of pottery were analyzed for determining chemical composition in order to establish their provenance. The potteries tested in the present research come from Himera and Pestavecchia archaeological sites. After digestion in microwave oven, the samples have been analyzed for fourteen minor elements (Ba, Cd, Co, Cr, Cu, Ga, Li, Mn, Ni, Pb, Sr, Ti, Tl, and Zn) and six major elements (Al, Ca, Fe, K, Mg, and Na). Chemical analysis was carried out by Inductively Coupled Plasma–Optical Emission Spectroscopy (ICP–OES). The most abundant minor elements are Cr, Ba and Ni. Cr concentration ranged from 66 to 3635 mg kg^{− 1}, Ba concentration ranged from 388 to 2677 mg kg^{− 1} and Ni concentration ranged from 35 to 1758 mg kg^{− 1}. The relative standard deviation (RSD) of the replicates on the concentrations of analyzed metals ranged from 0.07% to 14%.The aim of this study is to assign the local or non-local provenance of the examined potteries, in particular validating and clarifying archaeological hypothesis based on the simple visual examination and stylistic characterization of ceramic objects. Principal component analysis performed on the dataset, together with the application of cluster technique and non statistical analysis, allowed the identification of three main groups of samples and a lonely one (R 97). In particular, sample R 97 shows high Cr concentration (3635 mg kg^{− 1}) and high Ni concentration (1758 mg kg^{− 1}), typical of Corinthian pottery. The results of chemical analysis show that the stylistic features are not always sufficient to correctly identify the origin of a ceramic object.     

Determination of Si,Al, Ti,Fe and Zr in glass sand samples by 14 MeV neutron activation analysis

Fast neutron activation analysis technique was applied for the determination of Si, Al, Ti, Fe and Zr in glass sand rock samples. The samples and standards were irradiated with a mono-energetic neutron flux of 10⁸n · cm^– · s^–1. Pneumatic facility was used. The gamma activities from samples and standards were counted using a 30 cm³ Ge(Li) detector, with FWHM of 2.9 keV at 1.332 MeV, coupled to an on-line computer facility.