Quantitative analysis of sea-bed sediments from Eastern Black Sea by EDXRF spectrometry

Sea-bed sediments from Eastern Black Sea have been analyzed for their Fe, Ba and Sr contents using the methods of standard addition and energy dispersive X-ray fluorescence (EDXRF). Samples were prepared from powder sifted by a 200 mesh sieve. An annular 100 mCi²⁴¹Am radioactive source emitting 59.543 keV photons was used for excitation and a Ge(Li) detector, which has a 190 eV FWHM for 5.9 keV photons was used for intensity measurements. 2048 channels of the MCA are employed for 20 or 30 min. Dried and ground sea-bed sediments are found to contain 2.95–7.50% Fe, 0.032–0.268% Ba and about 73–273 ppm Sr. These results agree with those obtained via atomic absorption methods.     

Correction equations of coincidence summing using75Se radionuclide in the efficiency of HpGe detector

Correction equations of the coincidence-summing effect for efficiencies of HpGe detector based on the decay scheme were developed by considering the summing up to triple coincidence. The correction equations which do not dependent on the kind of the Ge detector are very useful for efficiency calibrations of a Ge detector in the energy region from 60 to 400 keV by using⁷⁵Se radionuclide even with very short source-to-detector distances.     

Elemental uptake of radish grown near a Municipal Solid Waste dumping site by EDXRF

Radish plant was collected along with root and soil from the nearby area of a Municipal Solid Waste dumping site of the metropolitan city of Kolkata, West Bengal, India and analyzed for a wide range of elements using the EDXRF technique with a ¹⁰⁹Cd point source and a Si(Li) detector. The samples comprized of the root-soil, root and leaves. For quality control purposes, NIST standard reference material (SRM) 1648 Urban Particulate Matter had also been analyzed using the same procedure as for the samples. Concentrations of elements with X-ray energies in the range of 3–20 keV in the soil around the root and their uptake pattern by the root and the leaves have been estimated.     

Determination of low-level 54Mn in soils by ultra low-background gamma-ray spectrometry after radiochemical separation

An analytical method was developed for the measurement of low-level ⁵⁴Mn in soil sample by ultra low-background g-ray spectrometry after radiochemical separation. The method consists of decomposition of sample by a mixture of HNO₃ and HF, dissolution by HNO₃, precipitation as hydroxide, solvent extraction with diisopropyl ether and anion exchange. Finally, for purification of Mn it was precipitated as MnO₂ by adding KClO₃. ⁵⁴Mn in the precipitate was measured by ultra low-background well-type Ge detector at Ogoya Underground Laboratory. Measurements of ⁵⁴Mn using 30-200 g of soil samples from the JCO grounds were successfully performed by the present method. The minimum detectable activity of ⁵⁴Mn was about 0.01 dpm (0.2 mBq) for a 7-day counting period.     

Standardless energy-dispersive X-ray fluorescence analysis using primary radiation monochromatized with LiF(200) crystal

Energy-dispersive X-ray fluorescence spectrometer (EDXRF) with primary radiation monochromatized by LiF(200) crystal was developed. In the constructed spectrometer, the radiation from the Ag target X-ray tube operated at 50 kV and 40 mA excites the secondary target (Cu, Se, Zr or Mo). The characteristic radiation (Cu K_α, Se K_α, Zr K_α or Mo K_α) of the target is monochromatized with LiF(200) crystal and excites elements in the analyzed sample. The X-ray spectra are collected by thermoelectrically cooled Si-PIN detector with resolution of 145 eV at 5.9 keV. The pinhole collimator placed in front of the X-ray detector allows reducing size of the analyzed area. Quantitative analysis is performed using standardless fundamental parameters (FP) method. Because sample is excited using highly monochromatized radiation, the calculations are much simpler and analysis error resulting from uncertainty of X-ray tube spectral distribution is completely eliminated. Moreover, EDXRF system allows obtaining very low background and appropriate secondary target can be selected for the best excitation of the determined elements and to avoid overlapping of the analyte peaks with characteristic radiation originating from the secondary target. The FP calculations were verified using several certified reference materials of stainless steel. The spectrometer was used for nondestructive analysis of mono- and polycrystals of selenide spinels of general formula M_xN_yCr_zSe₄ (where M, N are Cu²⁺, Zn²⁺, Cd²⁺, Mn²⁺, Ge²⁺, Ni²⁺, V³⁺, Sb³⁺, Ga³⁺). The results from EDXRF were compared with those obtained by means of the wavelength-dispersive X-ray fluorescence spectrometry (WDXRF).     

Performance of a gaseous detector based energy dispersive X-ray fluorescence imaging system: Analysis of human teeth treated with dental amalgam

Energy dispersive X-ray fluorescence (EDXRF) imaging systems are of great interest in many applications of different areas, once they allow us to get images of the spatial elemental distribution in the samples. The detector system used in this study is based on a micro patterned gas detector, named Micro-Hole and Strip Plate. The full field of view system, with an active area of 28 × 28 mm² presents some important features for EDXRF imaging applications, such as a position resolution below 125 μm, an intrinsic energy resolution of about 14% full width at half maximum for 5.9 keV X-rays, and a counting rate capability of 0.5 MHz. In this work, analysis of human teeth treated by dental amalgam was performed by using the EDXRF imaging system mentioned above. The goal of the analysis is to evaluate the system capabilities in the biomedical field by measuring the drift of the major constituents of a dental amalgam, Zn and Hg, throughout the tooth structures. The elemental distribution pattern of these elements obtained during the analysis suggests diffusion of these elements from the amalgam to teeth tissues.     

EDXRF analysis of some samples of cigarette paper

The effects of tobacco on human health have been widely investigated and documented However, there are not too many specific reports on the potential risk associated to the presence of metals in the paper employed for cigarettes fabrication Even more, there is a lack of national and international norms in this respect. Otherwise, in the literature INAA appears as the unique method for wrapping paper analysis. Therefore, without a nuclear reactor available at the National University of Mexico (UNAM), EDXRF was selected with the aim to explore the possibility to apply this method, instead of INAA, to the analysis of wrapping paper assuming this task, at the beginning, as a supplement to a previous research which was recently presented (2005).¹ The analytical work was developed on the wrapping paper of eight of the most known marks of cigarettes in Mexico, in two non-destructive stages: a first survey, by the classical technique of energy dispersive X-ray fluorescence (EDXRF), used a 1 11 GB qradiation source of ²³⁸Pu and a SiLi detector. In the absence of standard reference materials for cigarette’s paper, the SRM-1832 and 1833 were required for calibration, a fiberglass air filter was used as a secondary standard. The second stage was performed in a spectrometer TX-2000, anode of Mo, quantification software EDXRF32 (fundamental parameters). This paper presents a comparison of the obtained values with those found in the literature. The results show that the EDXRF method, in the Mo tube version, has the adequate precision and detection limits for the analysis of wrapping paper.     

High-resolution gamma spectrometry for measurement of transuranic radionuclides: A comparison of a low axial length-to-diameter coaxial HPGe detector versus a planar HPGe detector

A comparison of an HPGe planar detector and an HPGe coaxial detector, both with short length-to-diameter ratios, provides empirical evidence for the advantage of the coaxial configuration in measurements of actinide radionuclides. The principal advantage is related to the lower capacitance of a coaxial detector relative to that of a planar detector, both with large active frontal areas. In addition, the higher interaction probability (efficiency) of Ge versus Si underscores the advantages of Ge for measurements of samples with -ray energies from 5 to 200 keV (²³⁵U and²⁴¹Pu). The advantages are also dependent on the presence of other higher-energy -rays collimated versus diffuse-sample geometry, and (for bioassay applications) the intervening scattering mediums of bone and tissue.     

Determination of rare-earth eleemnts in rock samples by neutron activation analysis

A Ge(Li) detector combined with cation exchange separation has been used for the determination of 12 rare-earth elements (La, Ce, Nd, Sm, Eu, Gd, Tb, Ho, Er, Tm, Yb, and Lu) in rock samples by neutron activation analysis. After purification by the conventional hydroxide-fluoride precipitation, the rare-earth elements are separated into two fractions, light (La-Tb) and heavy (Ho-Lu), by EDTA cation exchange, and the γ-activities of the two fractions are measured by a Ge(Li) detector. The heavy rare-earths, such as Ho, Er, and Tm, can be easily γ-counted without serious interference from the intense Compton background and photopeaks due to the light rare-earths such as¹⁴⁰La,¹⁵³Sm,¹⁵²Eu, and¹⁶⁰Tb. The chemical yields (60%) for the individual rare-earths are determined by a reactivation technique. The results obtained for the U.S. Geological Survey standard rocks G-1 and W-1 are compared with the previously reported data.     

Analyse par spectrometrie gamma directe des produits de fission de235U

The γ-spectra of fission products of²³⁵U are analysed by a Ge(Li) detector after colling times of 3, 7 and 110 hrs. The possibility of the use of these results is demonstrated for measuring the mass distribution. Some preliminary values for the fission of²³²Th by 14 MeV neutrons are given.      

Measurement of radioactive samples in Marinelli beakers by gamma-ray spectrometry

Radioactivity measurement of environmental samples is frequently assayed by gamma-ray spectrometry using Marinelli beakers. In this work, self-absorption and coincidence summing effects arising in activity measurements for Marinelli beaker geometry have been studied with a Ge detector. Three types of Marinelli beakers which have capacities of 450 mL, 1 L, and 2 L were developed. Self-attenuation effects for density variation of radioactive samples in each type of the Marinelli beakers were measured as a function of gamma-ray energy, and also the results were compared with calculated values by mathematical model. Meanwhile, the coincidence summing effects of¹²⁵Sb and¹⁵⁴Eu nuclides were obtained from the determination of the full-energy peak and total efficiencies for a Ge detector.     

The Chemistry of GALLEX—Measurement of Solar Neutrinos with a Radiochemical Gallium Detector

In the GALLium Experiment, GALLEX, low-energy solar neutrinos produced in the main hydrogen fusion reaction inside the Sun are being counted for the first time in a radiochemical gallium detector. In this way, the theories about stellar structure may be verified and the question of the existence of a neutrino rest mass be brought closer to a solution. The experiment is being carried out with international collaboration at the Gran Sasso underground laboratory (LNGS) in the Abruzzi mountains in Italy. In this paper we survey the planning, construction and initial experimental operation of the gallium detector, paying special attention to the chemical aspects of the experiment. The chemical problem to be solved is the separation of very few ⁷¹Ge atoms from 100 metric tons of a highly concentrated GaCl₃ solution acidified with hydrochloric acid. In addition, these Ge atoms must be isolated and converted into germane, GeH₄, for low-level counting of ⁷¹Ge in a gas proportional counter. After extensive preparatory work to meet the extreme requirements of the experiment, the first results have now become available.     

Measurement of the radioactivity of238U,232Th,226Ra,137Cs and40K in soil using direct Ge(Li) γ-ray spectrometry

Radioactivity of the nuclides²³⁸U(²³⁵U),²³²Th,²²⁶Ra,¹³⁷Cs and⁴⁰K was measured in soil by direct -ray spectrometry using Ge(Li) detector. Relative laboratory method was used. Soil was dired, powdered, sieved and put into hemetically sealed container. CCRMP certified reference materials and compounds of the above nuclides mixed with fine quartz sand were used as references. Five and four -lines were used for the determination of²³²Th and²²⁶Ra, respectively, to obtain more accurate results. The most significant interferences, caused by the limited energy resolution of the detector, were resolved. In the case of ordinary soils, using one day duration of measurement and 1 kg mass of soil,²³²Th,²²⁶Ra and⁴⁰K can be determined with less than 10% relative random error. Elevated concentrations of²³⁸U(²³⁵U) and²²⁶Ra were observed in soil samples collected around a coal-fired power plant in Ajka town, Hungary.     

Determination of selenium in animal tissue samples using radioisotope induced X-ray fluorescence

A summary of sources of background affecting gamma-ray spectrometers and methods for eliminating each are discussed, along with practical cost/benefit ratios. Background contributed by samples generally defines practical levels for system background. The practical bottom line can be obtained for relatively modest costs. A realistic bottom line is attained in underground systems when the major contributions to the background come from cosmogenically produced⁶⁸Ge and double-beta decay of⁷⁶Ge in the detector. The true bottom line is reached with isotopically enriched detectors that eliminate these two chemically inseparable radioactive impurities. Data from isotopically enriched detectors are presented.     

Gamma-spektroskopisches Verfahren Zur Verfolgung von Zr−Hf-Trennungen

A quantitative γ-spectroscopic method for the persecution of Zr-Hf separation is described. The nuclides⁹⁵Zr and^175+181Hf are used as tracer. Difficulties caused by the presence of the radioactive daughter⁹⁵Nb are avoided by the application of a Ge(Li) detector. The simultaneous determination of Zr and Hf is possible over a wide range of concentration.      

Boron in natural waters by atomic absorption spectrometry with electrothermal atomization

Rapid scanning of numerous rock samples when prospecting for uranium and thorium ores can be facilitated by using the shorter-lived nuclides. The samples are activated during short epithermal neutron irradiations and the 20-min activities of ²³⁹U and ²³³Th are observed instrumentally with a small Ge(Li) detector. The detection limits for uranium and thorium are less than 1 ppm and 20 ppm, respectively.     

The determination of bromine in dry biological material by instrumental neutron activation analysis

Procedures for the determination of bromine by the reactions⁸¹Br(n, γ)⁸²Br (T=35.4 h) and⁷⁹Br(n, γ)^80mBr (T=4.4 h). In the case of⁸²Br a flat coaxial Ge(Li) crystal is used to measure the 619 keV photopeak. For^80mBr a planar Ge(Li) detector is applied to measure the 39 keV γ-ray. The agreement between the data obtained with both techniques for some Standard Reference Materials is satisfactory.     

Analysis of nuclear materials by energy dispersive X-ray fluorescence and spectral effects of alpha decay

Energy dispersive X-ray fluorescence (EDXRF) spectra collected from alpha emitters are complicated by artifacts inherent to the alpha decay process, particularly when using portable instruments. For example, ²³⁹Pu EDXRF spectra exhibit a prominent uranium L X-ray emission peak series due to sample alpha decay rather than source-induced X-ray fluorescence. A portable EDXRF instrument was used to collect qualitative spectra from plutonium and americium, and metal alloy identification was performed on a Pu-contaminated steel sample. Significant alpha decay-induced X-ray fluorescence peaks were observed in spectra obtained from the plutonium and americium samples due to the ²³⁵U and ²³⁷Np daughters, respectively. The plutonium sample was also analyzed by wavelength dispersive XRF (WDXRF) to demonstrate that alpha decay-induced X-ray emission has a negligible effect on WDXRF spectra.     

14.8 MeV neutron activation cross-sections for (n,p) and (n, α) reactions of some rare earth nuclides

The activation cross-sections for sixteen (n, p) and (n, α) reactions on rare earth nuclides were measured at 14.8 MeV neutron energy. A Ge(Li) detector was used for the radioactivity measurements. The measured cross-sections are compared with the semi-empirical predictions of LEVKOVSKII³ and BAYHURST and PRESTWOOD.¹⁶     

Multi-element determination in sandstone rock by instrumental neutron activation analysis

Summary Instrumental neutron activation analysis (INAA) was used for the qualitative and quantitative analysis of sandstone samples of Aswan area, in South Egypt. The samples were properly prepared together with standards and simultaneously irradiated by a neutron flux of 7 ^. 10¹¹ n ^. cm^-2.s^-1. in the TRIGA research reactor facilities in Mainz. The gamma-spectra from a hyperpure germanium HPGe detector were analyzed. The present study provides the basic data of elemental concentrations of a sandstone rock. The following elements have been determined: Na, K, Fe, Sc, Cr, Co, Zr, Ce, La, Nd, Sm, Eu, Yb, Lu, Hf, Ta, Th and U. Energy dispersive X-ray fluorescence (EDXRF) was used for comparison and to detect elements which can be detected only by this method.