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.     

Mercury analysis in environmental samples by EDXRF and CV-AAS

The analysis of total Hg in various environmental matrices was investigated using energy dispersive X-ray fluorescence (EDXRF) for both powdered and digested samples and cold vapor atomic absorption (CV-AAS) for digested samples. Several microwave decomposition procedures were evaluated with respect to the determination of Hg by CV-AAS and EDXRF. The use of different acid mixtures, microwave power settings and decomposition times were compared as well as the analysis on wet and freeze-dried samples. A set of standard reference samples were used to evaluate the procedures: NBS Citrus leaves (1572), NRC Pine needles (1575), NRC Dogfish muscle tissue (DORM-2), NRC Dogfish liver tissue (DOLM-2), BCR Human hair (397), BCR Coking coal (181) and NRC Marine sediment (PACS-1). An H₂SO₄/HNO₃/H₂O₂ acid mixture was found to be optimal for the complete mineralization and digestion of biological samples for Hg by CV-AAS whereas for EDXRF both the HNO₃/H₂O₂ and H₂SO₄/HNO₃/H₂O₂ acid mixture gave good results. The detection limit of EDXRF could significantly be decreased (from 0.2 μg/g to 0.058 μg/g) by performing the analysis with digested samples. A good agreement was obtained between CV-AAS and EDXRF analysis. The obtained results were also in good agreement with certified values. The methods were applied to environmental samples (coal, trees, leaves, spinach, fish, sediments) and human hair in a coal mining area and in places where they use coal for cooking in Vietnam. Received: 24 February 1997 / Revised: 13 June 1997 / Accepted: 18 June 1997     

Capabilities of elemental analysis by EDXRF for geochemistry

Elemental analyses of 10 geological samples from Morocco and some Standard Reference Materials were performed by Energy Dispersion X-Rays Fluorescence, Wavelength Dispersion X-Rays Fluorescence and Neutron Activation Analysis techniques in order to assess the accuracy and sensitivity of the concentrations determined with regard to requirements in geochemical exploration. The possibilities of utilization of EDXRF as an appropriate and economic technique for the analysis of various elements which are important in interpretation of geochemical data were evaluated.     

Determination of selenium in soil by hydride generation AAS

Hydride generation AAS was applied for the determination of total selenium in soil. The influence of various anions and cations present in the sample solution on the generation of selenium hydride was investigated. Special attention was paid to the wet oxidation procedure for the sample dissolution. The proposed procedure involves microwave sample preparation by using a mixture of H₂O₂/HNO₃/H₂SO₄. The accuracy of the procedure was checked by the analysis of the standard reference material Buffalo River Sediment (SRM-2704, NIST). Satisfactory agreement of the results obtained with the values reported was achieved. The detection limit of the procedure was 25 ng Se/g of soil. The relative standard deviation of the measurements varied from 5.5% for SRM-2704 up to 10% for the real soil samples. Received: 20 January 1997 / Revised: 24 February 1997 / Accepted: 1 March 1997     

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.     

Some aspects of chemical analysis of isolates by AAS

The paper describes some practical elements of atomic absorption spectrometry applications in the analysis of phase isolates. Attention was paid to the optimization of measuring conditions. It is pointed out that less sensitive analytical lines are more profitable. This paper presents the ranges of their practical application. The results of chemical analyses of the phase isolates are presented together with the morphological changes of the phase precipitations at different ageing temperatures.Dedicated to Professor Günther Tölg on the occasion of his 60th birthday     

Trace analysis of gallium arsenide by graphite furnace AAS

Summary Crystalline and powdered gallium arsenide samples are analysed by graphite furnace AAS. The sample is dissolved in hydrochloric acid and bromine, ammonium chloride as matrix modifier is added and the matrix elements are selectively evaporated as chlorides and bromides in the graphite tube of the atomizer before the atomization step. The temperature programs are optimized. The accuracy of the results was checked by recovery tests and by ICP-OES. The detection limits (g/g) are 0.1 (Ca, Fe), 0.05 (Zn, Pb), 0.03 (Mg), 0.01 (Al, Ni, Cu), 0.005 (Co), 0.002 (Cr) and 0.001 (Mn).

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Spurenanalyse von Galliumarsenid durch Graphitrohr-AAS

     

Study of natural and ion exchanged vermiculite by emanation thermal analysis,TG, DTA and XRD

Emanation thermal analysis (ETA), thermogravimetry, DTA and XRD were used in thermal characterization of natural vermiculite (Santa Olalla, Huelva, Spain) and of Na^+- and - exchanged vermiculite samples during heating in air in the range 25-1100°C. A good agreement between the results of these methods was found. Changes in the radon release rate measured by ETA, which reflected the decrease and collapse of the interlayer space after the release of water as well as the formation of new crystalline phases were evaluated using a mathematical model. The model used for the evaluation was found suitable for the quantitative characterization of microstructure changes during in situ conditions of heating of vermiculite samples. This revised version was published online in July 2006 with corrections to the Cover Date.     

Formation of protein-birnessite complex: XRD, FTIR, and AFM analysis

Limited information is available on formation chemistry of enzyme-Mn oxide complexes. Adsorption isotherm of protein molecules (tyrosinase) on birnessite (delta-MnO(2)) at pH 6.0 and room temperature (23 degrees C) was of H type, indicating a very high affinity of the enzyme protein molecules to the birnessite mineral surfaces. After thorough washing of the protein-mineral complex with deionized-distilled water, up to 89% of adsorbed protein molecules remained bound to the mineral surfaces. When a high amount of the protein was immobilized, the X-ray diffractogram shows a significant decrease in the intensity of characteristic d-spacings of birnessite. No shift to higher values of the d-spacings of protein-birnessite complex was observed, indicating that the enzyme molecules were not intercalated in the mineral structure but immobilized at the external surfaces and the edges of the mineral oxide. By comparison to the free enzyme, infrared absorption spectra of the protein-birnessite complexes show a shift by up to 11 cm(-1) to lower frequencies in the absorption bands characteristic of amide I and II modes of the polypeptides chains. The mineral surfaces exerted some strain on the protein structure, resulting in an alteration of the protein molecular conformation after binding to the mineral colloid surfaces. In the free state, the globular protein molecules had a spheroid shape with an average cross-sectional diameter of 70+/-6 nm. The unfolding and flattening of the protein molecules after immobilization is clearly shown in atomic force micrographs. Compared to the tyrosinase-birnessite complex, similar FTIR spectra and atomic force micrographs were observed for the pure protein, bovine serum albumin (BSA), after immobilization on birnessite. The information obtained in this study is of fundamental significance for understanding birnessite as an adsorbent of biopolymers and the catalytic role of the enzyme-birnessite complex.     

Study on the mineral extraction of legume and grass species from various soil types, by instrumental neutron activation analysis

Instrumental neutron activation analysis (INAA), followed by gamma-ray spectrometry, was used to determine the concentration of K, Ca, Mg, Na, Zn, Fe, Mn, Mo, Co, Cr, La, Eu and Th in six species of legumes and three species of grasses. Each species of forage was cultivated on two differet oxisols, that is, a red yellow Latossol and a dark red Latossol, with the aim of comparing the influence of the soils in the mineral extraction. Besides, on each kind of soil, two different limestone concentrations were used in order to verify how the soil pH correction could influence the elemental absorption in each species, and at the same time; to search for an optimum value of limestone concentration for each soil.     

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.     

Assessing soil pollution from a municipal waste dump in Islamabad, Pakistan: a study by INAA and AAS

INAA and AAS techniques have been employed to determine 40 elements in soil of a municipal waste dump in sector H-11, Islamabad. Background soil was also analyzed to study the extent of contamination of the dump site soil. Most of the major elements in these soils represented the geochemical composition of the soil in this area. The enrichment factors for quantified elements identified high Sb and Mg contents that could be attributed to the presence of PET and food materials in the waste. Geo-accumulation Index (I _geo), Pollution Index (PI) and the Integrated Pollution Index (IPI) have also been calculated for all elements. The values for these indices show that municipal waste has distorted the soil ambiance and the soil of waste dump site is slightly to moderately polluted as compared to the background soil. The dump soil was found to be moderately polluted by the elements Ba, Br, Ga, Rb, Zn, Ni and Pb. Significantly high Cu, Mg and Sb contamination was observed for the waste soil that is likely to pose an environmental issue if current waste disposal procedures are continuously employed.     

Investigation of uptake processes in a soil/mushroom system by AES and AAS methods

Investigations were carried out to explore how much Cd, Cs, Hg, Se, Ni and Pb trace elements cultivated mushrooms take up of the amount previously put into their soil. The intake of elements differs considerably to the extent that: on the one hand, mushrooms might be observed to behave practically as a filter for Mn, Ni and Pb; and on the other hand they accumulate Hg, Cd and Cs. The way manganese gets into the fruit body was also investigated and, in addition, the element effect on the increase of production was measured. All the experiments were carried out in the knowledge of the significant role manganese has in the decomposition of cellulose.     

Thermal and XRD analysis of Egyptian galena

Galena is the principal ore mineral for lead industry and the production of lead and its alloys. The industrial processing of galena includes its oxidized roasting to lead oxide, followed by reduction smelting of lead oxide agglomerate with coke in the blast furnace to commercial lead. The present work reports a thermal analysis study of oxidized roasting of Egyptian galena using a derivatograph. The reaction products were identified microscopically and by using a Siemens Crystalloflex diffractometer.     

In-line determination of U,Pu and Np in process streams by energy-dispersive X-ray fluorescence analysis (EDXRF)

A -ray source of 300 keV was used in order to excite the fluorescent K-radiation of the heavy elements which is only weakly absorbed in the walls of metal tubes. Thus, uranium can be determined quantitatively in solutions within tubes in the concentration range form 5 mg/l to 100 g/l. The influences of the energy and the activity of the radiation source, the geometrical arrangement, the thickness of the wall and the wall material have been investigated.     

XRD,TEM and thermal analysis of yttrium doped boehmite nanofibres and nanosheets

Yttrium doped boehmite nanofibres with varying yttrium content have been prepared at low temperatures using a hydrothermal treatment in the presence of poly(ethylene oxide) surfactant (PEO). The resultant nanofibres were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). TEM images showed the resulting nanostructures are predominantly nanofibres when Y-doping is less than 5%; in contrast Y-rich phases were formed when doping was around 10%. The doped boehmite and the subsequent nanofibres/nanotubes were analyzed by thermogravimetric and controlled rate thermal analysis methods. The boehmite nanofibres produced in this research thermally transform at higher temperatures than boehmite crystals and boehmite platelets. Boehmite nanofibres decompose at higher temperatures than non-hydrothermally treated boehmite.     

XRD,TEM and thermal analysis of Fe doped boehmite nanofibres and nanosheets

Iron doped boehmite nanofibres with varying iron content have been prepared at low temperatures using a hydrothermal treatment in the presence of poly(ethylene oxide) surfactant. The resultant nanofibres were characterized by X-ray diffraction (XRD), and transmission electron microscopy (TEM). TEM images showed the resulting nanostructures are predominantly nanofibres when Fe doping is no more than 5%; in contrast nanosheets were formed if Fe doping was above 5%. For the 10% Fe doped boehmite, a mixed morphology of nanofibres and nanosheets were obtained. Nanotubes instead of nanofibres were observed in samples with 20% added iron. The Fe doped boehmite and the subsequent nanofibres/nanotubes were analysed by thermogravimetric and differential thermogravimetric methods. Boehmite nanofibres decompose at higher temperatures than non-hydrothermally treated boehmite and nano-sheets decompose at lower temperatures than the nanofibres.     

Qualitative and quantitative analysis of oxytetracycline by near-infrared spectroscopy

Near-infrared (NIR) spectroscopy, in combination with chemometrics, enable the analysis of raw materials without time-consuming sample preparation methods. The aim of our work was to estimate critical parameters in the analytical specification of oxytetracycline, and consequently the development of a method for quantification and qualification of these parameters by NIR spectroscopy. A Karl Fischer (K.F.) titration to determine the water content, a colorimetric assay method, and Fourier transform-infrared (FT-IR) spectroscopy to identify the oxytetracycline base, were used as reference methods, respectively. Multivariate calibration was performed on NIR spectral data using principal component analysis (PCA), partial least-squares (PLS 1) and principal component regression (PCR) chemometric methods. Multivariate calibration models for NIR spectroscopy have been developed. Using PCA and the Soft Independent Modelling of Class Analogy (SIMCA) approach, we established the cluster model for the determination of sample identity. PLS 1 and PCR regression methods were applied to develop the calibration models for the determination of water content and the assay of the oxytetracycline base. Comparing the PLS and PCR regression methods we found out that the PLS is better established by NIR, especially as the spectroscopic data (NIR spectra) are highly collinear and there are many wavelengths due to non-selective wavelengths. The calibration models for NIR spectroscopy are convenient alternatives to the colorimetric method and to the K.F. method, as well as to FT-IR spectroscopy, in the routine control of incoming material.     

Concentrations of Fe, Cu and Zn in rum by EDXRF using APDC preconcentration

Ten rum (aguardente) samples commercialized in Piracicaba region, São Paulo State, Brazil Southeast, were analysed by energy-dispersive X-ray fluorescence (EDXRF) using ammonium pyrrolidinedithiocarbamate (APDC) preconcentration in order to determine Fe, Cu and Zn concentrations. The effect of sucrose (2%) was also studied in this methodology, using a multielemental standard solution (40% ethanol). Copper concentrations in two samples were higher than the value allowed by Brazilian law. Limits of detection for these elements were in the ng^.ml^-1 range.