Trace element study of kidney stones from subjects belonging to stone belt region of India

Kidney stones obtained from six patients belonging to the stone belt region of India (Punjab) were analyzed for inorganic constituents using instrumental neutron activation analysis (INAA) and energy dispersive X-ray fluorescence (EDXRF) techniques. For INAA, samples were irradiated along with IAEA RM Soil 7 as reference standard in CIRUS reactor, BARC, Mumbai. Gamma activity of irradiated samples was measured using a 45% relative efficiency HPGe detector coupled to 8?k channel analyzer. EDXRF method was used for determination of concentration of Ca. The concentrations of ten elements namely Ca, Na, K, Mn, Co, Cr, Zn, Br, Sm and Cl, are reported and discussed.     

EDXRF as an analytical tool in art: Case studies from pigment identification and treatment assessment

Energy dispersive X-ray fluorescence (EDXRF) was employed for the identification of pigments decorating Hellenistic figurines, and the assessment of the efficiency of a treatment with barium hydroxide applied to stone. Elements present in the colored areas of the figurines, as well as the treated stone was identified by EDXRF. These data together with complementary information obtained by Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction analysis (XRD) led to the identification of several precious pigments. As far as the treatment efficiency is concerned, EDXRF analysis revealed that barium is unevenly distributed on the treated surface and reaches a maximum depth of 2.5 mm.     

EDXRF as an analytical tool in art: Case studies from pigment identification and treatment assessment

Energy dispersive X-ray fluorescence (EDXRF) was employed for the identification of pigments decorating Hellenistic figurines, and the assessment of the efficiency of a treatment with barium hydroxide applied to stone. Elements present in the colored areas of the figurines, as well as the treated stone was identified by EDXRF. These data together with complementary information obtained by Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction analysis (XRD) led to the identification of several precious pigments. As far as the treatment efficiency is concerned, EDXRF analysis revealed that barium is unevenly distributed on the treated surface and reaches a maximum depth of 2.5 mm.     

Studies of kidney stones using INAA,EDXRF and XRD techniques

Four kidney stones collected from patients being treated in the Advance Urology Centre of PGIMR, Chandigarh were characterized using instrumental neutron activation analysis (INAA), energy dispersive X-ray fluorescence (EDXRF) and X-ray diffraction (XRD) techniques. For INAA, samples were irradiated in tray rod facility of Dhruva reactor, Mumbai and pneumatic fast transfer system of KAMINI reactor, IGCAR, Kalpakkam. Radioactive assay was carried out using HPGe detector coupled to 8k channel analyzer. Elements determined in the samples by INAA are Zn, Sr, Co, Fe, Cr, Sc, Se, Na and Mn. EDXRF was used for the quantification of Ca. XRD patterns showed that three of the kidney stones are calcium oxalate stone and the other one is uric acid stone. The concentrations of trace elements in general were found to be higher in calcium oxalate stones and positive correlation was observed in the concentrations of Ca with Sr and Zn.     

Determination of Cr,Fe, Co,Ni, Cu,Zn, As and Pb in liquid chemical waste by energy dispersive X-ray fluorescence

A method for simultaneous determination of Cr, Fe, Co, Ni, Cu, Zn, As e Pb in liquid chemical waste using Energy Dispersive X-Ray Fluorescence (EDXRF) technique was evaluated. A small sample amount (200 μL) was dried on a 6.35 μm thickness Mylar film at 60 °C and the analyses were carried out using an EDXRF spectrometer operated with an X-ray Mo tube (Zr filter) at 30 kV/20 mA. The acquisition time was 300 s and the Ga element was utilized as internal standard at 25 mg/L for quantitative analysis. The method trueness was assessed by spiking and the detection limit for those elements ranged from 0.39 to 1.7 mg/L. This method is notable because it assists the choice of the more appropriated waste treatment procedure, in which inter elemental interference is a matter of importance. In addition, this inexpensive method allows a non-destructive determination of the elements from ₁₉K to ₉₂U simultaneously.     

Elemental analysis of Cu−Ni and Nd−Al alloys and, nickel and iron powders by energy dispersive X-ray fluorescence (EDXRF) technique

Energy dispersive X-ray fluorescence spectroscopy (EDXRF) has been used for elemental analysis of Cu−Ni alloy, neodymium aluminide, and iron and nickel powder. The preparation of Cu−Ni alloy and neodymium aluminide has been carried out by aluminothermic reduction of mixed oxides of copper and nickel and neodymium oxide respectively. Aqueous electrorefining technique has been followed for the preparation of iron and nickel powder using Fe−Ni alloy as anode. The determination of major and trace elements present in the Cu−Ni and, electrolytically refined nickel and iron has been accomplished by EDXRF using Cd¹⁰⁹ radioisotope source. In the case of Nd−Al alloy Am²⁴¹ radioisotope source has been used. The rapid and multielement analysis of the thermit product by EDXRF has aided in the appropriate variation of the charge constituents during the standardization of the optimum charge composition for Cu−Ni alloy. EDXRF analysis of electrolytically refined nickel and iron revealed heavy contamination of iron in nickel as compared to that of nickel in iron. Neodymium content has been found to be 67.68% in Nd−Al alloy.     

Energy dispersive X-ray fluorescence as a tool in biomedical analysis

Summary The energy dispersive X-ray fluorescence spectrometer (EDXRF) developped together with the Siemens Company (FRG) allows to perform rapid multi-elemental analysis of biological fluids without pretreatment of the samples. The performance of this technique and its features are reported in two different fields: blood analysis and pulmonary investigations. Blood and plasma analysis were performed for more than 2500 patients and a statistical treatment of the data lead to the normal concentrations of trace elements Se, Rb, Cu, Zn, Fe, Ca, Br, K. Toxic elements such as Hg or Pb and also drugs like Au and Pt compounds can be detected even after a long period after treatment. To illustrate the performance of the spectrometer we report the influence of Cis-Pt treatment on the trace element concentrations in plasma of patients with anemia.The EDXRF spectrometry was also used to investigate the inorganic composition of the broncho-alveolar lavage fluids. After determination of the normal concentration range, it was possible to characterize some typical pulmonary diseases due to occupational exposure. Some examples of detected pneumoconiosis and for some patients the presence in the alveoli of elements due to special medication (Amiodarone, Aurothiopropanol-sulfonate) are mentioned.Other fields are being investigated such as: follow-up of Mn dependent enzymes in neuronal and glial cells in culture; origin of lead in dental tissues or composition of lyophilized food powders. They will be briefly discussed.

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Energie-dispersive Röntgenfluorescenz in der biomedizinischen Analyse

     

Combined Semi-absolute FNAA and EDXRF in coal analysis

A combination of Semi-absolute Fast Neutron Activation Analysis (SFNAA) and Energy Dispersive X-ray Fluorescence (EDXRF) analysis has been employed to determine 35 inorganic elements in coals from four different mines across the minefields of Nigeria. A plot of certified against measured values of elemental constituents in a National Bureau of Standard coal reference material, SRM 1632 a, with a regression coefficient of r=0.894, is used to demonstrate the efficacy of this technique. With a complimentary application of the EDXRF technique, better precision is obtained for short-lived isotopes reducing the need for a more sophisticated transfer system and cyclic activation analysis in the situation under discussion.     

Quantitative multielemental analysis of titaniferous magnetites

Two representative titaniferous magnetite samples procured from Moulabhanj, Orissa, India have been studied by PIXE, EDXRF, Mössbauer spectroscopy, and XRD techniques. Major iron-bearing phases identified in the samples by Mössbauer spectroscopy and XRD are magnetite, hematite, ferrous ilmenite and ferric ilmenite. The Fe²⁺/Fe³⁺ ratio and the relative percentages of different minerals were determined from the resonance areas of Mössbauer spectra. Quantitative multielemental analysis was carried out by energy dispersive X-ray fluorescence (EDXRF) and proton induced X-ray emission (PIXE). Nineteen minor and trace elements have been quantified by EDXRF whereas by PIXE eighteen elements have been analyzed quantitatively. Concentrations of trace elements determined by EDXRF and PIXE were used in interpreting the physico-chemical condition of the depositional basin.     

Iron Forms Fe(II) and Fe(III) Determination in Pre-Roman Iron Age Archaeological Pottery as a New Tool in Archaeometry

This article presents studies on iron speciation in the pottery obtained from archaeological sites. The determination of iron forms Fe(II) and Fe(III) has been provided by a very simple test that is available for routine analysis involving the technique of molecular absorption spectrophotometry (UV–Vis) in the acid leachable fraction of pottery. The elemental composition of the acid leachable fraction has been determined by inductively coupled plasma optical emission spectrometry (ICP-OES). Additionally, the total concentration of the selected elements has been determined by X-ray fluorescence spectrometry with energy dispersion (EDXRF). The results of the iron forms’ determinations in archaeological pottery samples have been applied in the archaeometric studies on the potential recognition of the pottery production technology, definitely going beyond the traditional analysis of the pottery colour.     

Determination of tungsten in ores by energy dispersive X-ray fluorescence analysis

The possible determination of tungsten in low grade ores from Northern India, Rajasthan State has been explored by energy dispersive X-ray fluorescence analysis /EDXRF/ technique using radioisotope based excitation of W L X-rays and high resolution Si/Li/ detector system. Finely powdered ore has been diluted with optimal quantity of cellulose and converted into pellets to make it suitable for X-ray analysis after homogenization. The experiments have shown the minimum detectable limit of 33 ppm in diluted matrix. The results are compared with the spectrophotometric stannous chloride-thiocyanate method. EDXRF appears to be encouraging for routine and precise analysis of tungsten in low grade ores.     

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 TiO₂ 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 TiO₂ 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.     

Essential and trace element contents of some Nigerian medicinal plants

The energy-dispersive X-ray fluorescence (EDXRF) spectroscopy has been used for the determination of essential and trace elements" contents of some twenty Nigerian medicinal plants. The accuracy and precision of the technique were assured by analyzing the European Community Bureau Reference Standard BCR 62 (Olive Leaves). Fourteen elements, namely K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Se, Br, Rb, Sr were detected with toxic heavy metal such as Cd, As, Pb, Hg were detected in the samples. The ranges of elemental concentrations varied from 7.7^.10⁴ to 1.6 mg/kg in the herbs. The results show that many of these plants contain elements of vital importance for human metabolism and prevention and healing of diseases.     

Energy dispersive X-ray fluorescence analysis of gallstones

The elemental analysis of south Indian gallstones has been carried out using energy dispersive X-ray fluorescence (EDXRF) spectroscopy. A number of important elements including Fe, Cu, Zn, Br, and Pb were estimated from the EDXRF spectra. The results are presented and discussed.     

EDXRF versus INAA in a pollution control of soil

Summary Elemental concentrations of soil samples collected in the vicinity of a Romanian fertilizer plant were determined by EDXRF and long half-life INAA. Lower limits of detection, obtained for various elements in soil by EDXRF technique with radioactive excitation sources (²³⁸Pu and ²⁴¹Am) and a HPGe detector are presented. Spurious effects characteristic for Ge detector X-ray spectrometry are evaluated and discussed, and methods to overcome this drawback are suggested. Special care was taken to subtract from the spectra the Ge Ka     

Energy Dispersive X-Ray Fluorescence Analysis and X-Ray Microanalysis of Medieval Silver Coins

 Austrian medieval silver/copper coins were investigated at their surfaces by energy dispersive X-ray fluorescence analysis (EDXRF) and at the cross-sections by X-ray microanalysis in the scanning electron microscope (SEM/EDX) in order to estimate the error occurring when corroded objects of art and archaeology are analyzed on the surface by non-destructive methods. Additionally, Ag/Cu-standards were treated in diluted sulphuric acid and the depletion of copper on the surface was measured by EDXRF. By calculating the ratio of the Ag-K/Ag-L intensity the process of blanching could be studied.     

Analysis of low levels of rare earths by radiochemical neutron activation analysis

A procedure for the radiochemical neutron-activation analysis for the rare earth elements (REE) involves the separation of the REE as a group by rapid ion-exchange methods and determination of yields by reactivation or by energy dispersive X-ray fluorescence (EDXRF) spectrometry. The U. S. Geological Survey (USGS) standard rocks, BCR-1 and AGV-1, were analyzed to determine the precision and accuracy of the method. We found that the precision was ±5–10% on the basis of replicate analysis and that, in general the accuracy was within ±5% of accepted values for most REE. Data for USGS standard rocks BIR-1 (Icelandic basalt) and DNC-1 (North Carolina diabase) are also presented.     

Determination of zinc in ammoniacal ore leaching solutions by X-ray fluorescence spectrometry using a radioactive source

A method was developed for the fast determination of zinc in leaching solutions by radioisotope energy-dispersive X-ray fluorescence (EDXRF) spectrometry. The measured intensities were used to develop regression models for estimating the zinc concentration. The primary radiation was provided by the ²⁴⁴Cm radioisotope. Several experimental parameters including the saturation thickness and detection limit were determined. The advantages of the utilization of conditioning agents with elements of low atomic number such as nitric acid were established.     

Thickness measurement of semiconductor thin films by energy dispersive X-ray fluorescence benchtop instrumentation: Application to GaN epilayers grown by molecular beam epitaxy

The importance of thin films in modern high technology products, such as semiconductors, requires fast and non-destructive analysis. A methodology to determine the thickness of single layers with benchtop energy dispersive X-ray fluorescence (EDXRF) instrumentation is described and tested following analytical validation criteria. The experimental work was carried out on gallium nitride thin films epitaxially grown on sapphire substrate. The results of samples with layers in the range from 400 to 1000 nm exhibit a good correlation with the layer thickness determined by optical reflectance. Spectral data obtained using thin layered samples indicate the possibility to precisely evaluate layer thickness from 5 nm, with a low relative standard deviation (RSD < 2%) of the results. In view of the limits of optical reflectance for very thin layer determination, EDXRF analysis offers the potential for the thickness determination of such kind of samples.     

植物药抑制泌尿系结石形成的化学基础

植物药治疗泌尿系结石具有独特的疗效.本文综述了国内外植物药(泽泻,Phyllanthus niruri,Zeamays,Agropyron repens和Herniaria hirsute等)在体外模拟实验和动物实验中对泌尿系结石形成的影响,植物药抑制泌尿系结石形成的机制和化学基础是:植物药与钙离子发生配位,降低尿石盐的过饱和度;抑制一水草酸钙生长,诱导二水草酸钙形成;抑制晶体生长和聚集;可以保护尿路粘膜,防止晶体在肾上皮细胞上发生粘附;改变尿石形成促进剂和抑制剂的排泄量.