Study of ceramics from Brazilian slave quarters of the XVIII and XIX centuries by EDXRF and multivariate analysis.

This study refers to the archaeometric analysis of ceramic fragments found in archaeological excavations around slave quarters of Colégio dos Jesuítas and São Bento plantations, both located in Campos dos Goytacazes - RJ. The question whether handmade ceramics were produced by the slaves themselves or acquired through local trade networks is an open and important question in the African diaspora. Samples of clay sources and the ceramic fragments, were analyzed using the EDXRF technique with the aid of multivariate statistical analysis.

A low-cost portable system for elemental mapping by XRF aiming in situ analyses.

This work presents the development of a portable system that allows 2D elemental mapping of large areas (maximum of 35.0 × 35.0 cm2) by XRF. A measuring head, composed of an x-ray source and a detector, is mounted on a 3-axis stage with movement reproducibility better that 0.03 mm. The final elemental map resolution of 1.4 mm was experimentally determined in the best condition of collimation, and the same experiments indicate that the resolution is fully dominated by the x-ray beam spot size. The main goal of this new setup is to perform analyses of historical, archaeological and geological objects. Because it's lightweight, our setup has the potential to be of great utility for in situ analyses, given the great difficulty and high costs transporting the artifacts from the museum to a laboratory. The importance of this instrumentation is related to the need to identify the distribution of the chemical elements in large surface areas of cultural heritage objects by a nondestructive method.

Pigments analysis and gold layer thickness evaluation of polychromy on wood objects by PXRF.

The X-ray fluorescence technique by energy dispersion (EDXRF), being a multi elemental and non-destructive technique, has been widely used in the analysis of artworks and archeometry. An X-ray fluorescence portable equipment from the Laboratory of Applied Nuclear Physics of the State University of Londrina (LFNA/UEL) was used for the measurement of pigments in golden parts of a Gilding Preparation Standard Plaque and also pigments measurement on the Wood Adornment of the High Altar Column of the Side Pulpit of the Immaculate Conception Church Parish Sao Paulo-SP. The portable X-ray fluorescence PXRF-LFNA-02 consists of an X-ray tube with Ag anode, a Si-PIN detector (FWHM=221 eV for Mn line at 5.9 keV), a chain of electronics nuclear standard of X-ray spectrometer, a multichannel 8K, a notebook and a mechanical system designed for the positioning of detector and X-ray tube, which allows movements with two degrees of freedom from the system of excitation-detection. The excitation-detection time of each measurement was 100 and 500 s, respectively. The presence of elements Ti, Cr, Fe, Cu, Zn and Au was found in the golden area of the Altar Column ornament. On the other hand, analysis of the ratios for the intensities of Kα/Kß lines measured in the areas made it possible to explore the possibility of measuring the stratigraphies of the layers of pigments and to estimate the thickness of the same.

Portable XRF and principal component analysis for bill characterization in forensic science.

Several modern techniques have been applied to prevent counterfeiting of money bills. The objective of this study was to demonstrate the potential of Portable X-ray Fluorescence (PXRF) technique and the multivariate analysis method of Principal Component Analysis (PCA) for classification of bills in order to use it in forensic science. Bills of Dollar, Euro and Real (Brazilian currency) were measured directly at different colored regions, without any previous preparation. Spectra interpretation allowed the identification of Ca, Ti, Fe, Cu, Sr, Y, Zr and Pb. PCA analysis separated the bills in three groups and subgroups among Brazilian currency. In conclusion, the samples were classified according to its origin identifying the elements responsible for differentiation and basic pigment composition. PXRF allied to multivariate discriminate methods is a promising technique for rapid and no destructive identification of false bills in forensic science.

Committed effective dose determination in southern Brazilian cereal flours.

The health impact of radionuclide ingestion from foodstuffs was evaluated by the committed effective doses determined in eight commercial samples of South-Brazilian cereal flours (soy, wheat, cornmeal, cassava, rye, oat, barley and rice flours). The radioactivity traces of (228)Th, (228)Ra, (226)Ra, (40)K, (7)Be and (137)Cs were measured by gamma-ray spectrometry employing an HPGe detector of 66 % relative efficiency. The efficiency curve has taken into account the differences in densities and chemical composition between the matrix and the certified sample. The highest concentration levels of (228)Th and (40)K were 3.5±0.4 and 1469±17 Bq kg(-1) for soy flour, respectively, within the 95 % confidence level. The lower limit of detection for (137)Cs ranged from 0.04 to 0.4 Bq kg(-1). The highest committed effective dose was 0.36 µSv.y(-1) for (228)Ra in cassava flour (adults). All committed effective doses determined at the present work were lower than the International Atomic Energy Agency dose limit of 1 mSv.y(-1), to the public exposure.

Quantification of metals in river water using a portable EDXRF system.

This work identified, quantified, and presents results for metals in water using a portable energy dispersive X-ray fluorescence (EDXRF) system. It was possible to quantify the following range of concentrations in mg L(-1): Ca(0.043-0.021), Ti(0.137-0.014), Mn(0.052-0.008), Fe(1.66-0.035), Ni(0.012-0.010), Cu(0.010-0.007), Zn(0.070-0.007), and Pb(1.01-0.85). The final conclusion is that in 4h of field work it was possible to prepare, measure, and analyze 14 membranes.

Titanium dioxide determination in sunscreen by energy dispersive X-ray fluorescence methodology.

Nowadays there are many sun-protection cosmetics incorporating chemical and/or physical UV filters as active ingredients and there are no official methods to determine these kinds of compounds in sunscreen cosmetics. The objective of this work is to estimate TiO(2) concentration, without sample preparation, employing a portable energy dispersive X-ray fluorescence (EDXRF), aiming to estimate the sun protection factor (SPF) due to the physical barrier in sunscreen composition, and also identify the metals present in the samples. A portable EDXRF system was used for the analysis of fifteen commercial samples. It was also prepared three formulations estimated in FPS-30 using TiO(2) at 5%. Quantification was performed using calibration curves with standards from 1 to 30%. The physical barrier contribution in the SPF, associated to Ti concentration, was determined for all samples. The presence of some elements, like K, Zn, Br and Sr was detected in the sunscreen, identifying chemical elements that were not cited in the formulations. Three commercial samples were analyzed for total SPF determination and the result shows that the measured value is 10% lower than the nominal one.

Factorial design for Fe, Cu, Zn, Se and Pb preconcentration optimization with APDC and analysis with a portable X-ray fluorescence system.

Preconcentration of heavy metals in water with ammonium pyrrolydine dithiocarbamate (APDC) is a common practice in analytical chemistry. A literature review on this topic showed that several authors use this precipitation agent, but in different preconcentration conditions, conducting to divergent results. The objective of this work is to use factorial design to optimize the factors involved in the preconcentration process of heavy metals using APDC. Five factors were studied: sample volume, solution pH, APDC concentration, APDC volume and stirring time. The assays were performed by energy dispersive X-ray fluorescence (EDXRF). The values for detection limits within 95% confidence level, in microg L(-1), were: Fe (6.0+/-0.1), Cu (4.0+/-0.1), Zn (2.0+/-0.1), Se (4.0+/-0.1) and Pb (5.0+/-0.1). The value for quantification limit for the five elements was 20 microg L(-1), with 3% deviation. Multi-element standard solutions were prepared. Precipitation procedure was applied in the spiked solutions and the samples were filtered in cellulose ester membrane for quantification measurements. The optimum values obtained were 300 mL of sample solution, pH 4, 1 mL of 2% APDC and 10 min of stirring time. The concentration results obtained for the validation measurements were satisfactory for in situ survey employing a portable instrument.

Self-absorption correction for gamma spectrometry of powdered milk samples using Marinelli beaker.

Self-absorption was measured for the activity calculation of the 1460.8 and 2614.47 keV lines of the 40K and the 208Tl, respectively, in powdered milk samples. Five Marinelli beakers were prepared with powdered milk in different degrees of compaction and the spectra were measured with an HPGe detector. The detection efficiency versus density was obtained and the self-absorption correction factors versus density were calculated for powdered milk. The results obtained show that this factor must be considered in the calculations of activities.