Simultaneous determination of low Z elements in barium borosilicate glass samples by in situ current normalized particle induced gamma-ray emission methods

Particle induced gamma-ray emission (PIGE) method using 4 MeV proton beam was utilized to analyze two types of barium borosilicate glass (BaBSG) samples for quantification of concentrations of low Z elements. The in situ current normalization method was applied in the analysis of eight samples containing varying concentration of F along with Si, B and Na. Charge normalized PIGE method was applied to determine concentrations of above low Z elements including Li and Al in samples having simulated nuclear waste from reprocessing of thoria spent fuel. Synthetic samples and NIST SRMs were used for method validation.     

Determination of fluorine concentrations in soil samples using proton induced gamma-ray emission

A non-destructive, in situ current normalized particle induced gamma-ray emission methodology has been standardized for quantification of fluorine (F) in soil samples from Punjab state, India. The samples were irradiated using 4 MeV proton beam from the Folded Tandem Ion Accelerator at BARC, Mumbai. The gamma rays of energies 197 and 478 keV arising from ¹⁹F(p, p′γ)¹⁹F and ⁷Li(p, p′γ)⁷Li nuclear reactions were measured using high resolution gamma-ray spectrometry. The concentration of fluorine in soil samples was found to vary between 414 and 5,746 mg kg^?1.     

A simple and sensitive particle induced gamma-ray emission method for non-destructive quantification of lithium in lithium doped Nd2Ti2O7 ceramic sample

A particle induced gamma-ray emission method using proton beam in conjunction with in situ current normalization approach was standardized for non-destructive determination of low Z element lithium and was applied for quantification of Li in lithium doped neodymium dititanate (Nd₂Ti₂O₇) ceramic sample. Thick pellets of heat treated samples, their precursors and Li standards were prepared separately by homogeneously mixing with cellulose and fixed amount of F used for in situ current normalization. For validation of the method, four synthetic samples were also analyzed. Samples and standards were irradiated with 4?MeV proton beam (~5?nA current) from folded tandem ion accelerator (FOTIA) BARC, Mumbai. Characteristic ??-rays of 478?keV from ⁷Li to 197?keV from ¹⁹F were measured by high resolution ??-ray spectrometry. The Li concentrations determined in the six samples were in the range of 0.29?C0.85?wt%. The Li contents in heat treated samples gave the idea about loss of Li compared to their precursors.     

Rapid determination of fluorine in solid samples

A rapid method for the determination of fluorine in various matrices of geochemical and environmental interest is described. After fusion with NaOH, the sample is dissolved by means of tiron (= pyrocatechol-3,5-disulfonic acid, disodium salt), which acts both as buffer substance and as superior masking agent for cations exhibiting strong complexes with fluoride, e.g. Al, Fe, Ti etc. The final determination is done by means of the fluoride sensitive electrode without further separation.The applicability of the method has been checked for various silicates, bauxite, phosphates, soils, coal and plant material. A detection limit of 10 µg/g can be achieved, which is sufficient in many cases. The overall precision is better than ±10%.Dedicated to Prof. Dr.K. L. Komarek on occasion of his 60th birthday.     

Analytical use of alpha-source induced gamma-ray emission

Summary A non-destructive multi-element method based on nuclear reactions and Coulomb excitation induced by alpha-sources and the measurement of prompt gamma-rays is described. The method is suitable for light and medium Z elements and is particularly sensitive to light elements. The experimental set-up necessary for the prompt measurements is quite simple. With 0.34 mCi ²⁴¹Am source, the sensitivity of the method is discussed for the light elements Li, Be, F and Na. The influence of sample size, air pressure etc. on the thick target yield has been investigated. Monte-Carlo calculations have been performed to study the modification of the isotropic behaviour of the alpha-source due to the protective covering and to calculate the average energy loss. The lithium determination in some minerals has been carried out.

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Analytische Anwendung der -induziertcn -Emission

Zusammenfassung Eine zerstörungsfreie Multielement-methode, die auf Kernreaktionen und Coulombanregung induziert durch -Quellen beruht, sowie die Messung prompter -Strahlung werden beschrieben. Die Methode eignet sich für leichte und mittelschwere Elemente und ist besonders empfindlich bei leichten Elementen. Der für Promptmessungen notwendige experimentelle Aufbau ist recht einfach. Die Empfindlichkeit der Methode bei Benutzung eines 0,34 mCi starken ²⁴¹Am-Präparats wird für die leichten Elemente Li, Be, F und Na diskutiert. Der Einfluß von Probengröße, Luftdruck usw. auf die Ausbeute eines dicken Targets wurde untersucht. Monte-Carlo-Rechnungen wurden ausgeführt, um die Modifizierung der isotropen Abstrahlung der Quelle durch deren Schutzabdeckung zu studieren und um den mittleren Energieverlust zu erhalten. Eine Li-Bestimmung in einigen Mineralen wurde durchgeführt.

     

Prompt gamma-ray neutron activation analysis for multi-element determination in sediment samples

A facility for the irradiation of internal targets has been installed at the research reactor FRG-of the GKSS Research Center. Thermal-neutron induced prompt gamma radiation was detected by pair spectrometer. With this experimental arrangement concentrations of the major and mino elements Na, Al, Si, K, Ca, Ti, Mn, Fe, Zn, Cl, and S, as well as of the trace constituents Cr Ni, Cu Cd, and Hg of samples from a sediment core of the Elbe River could be determined. The results indicate, that prompt gamma-ray neutron activation analysis (PGNAA) is a powerful instrumental tool for a complete characterization of the main sediment constituents and for the detection of the trace elements Cd and Hg which are of considerable ecological relevance.     

Precise,non-destructive determination of fluorine by 14-MeV neutron activation analysis

A procedure is described for the precise determination of fluorine in organic and metal-organic compounds by 14-MeV neutron activation analysis using the reaction: ¹⁹F(n,2n)¹⁸F (β +, t_{$\text{1}\text{2}$} = 110 min).A relative standard deviation of better than ±0.5% is achieved by irradiating samples and standard simultaneously. Uniform neutron exposures were ensured by rotating the samples during irradiation. Positron emitters of short half-life are allowed to decay before counting. In metal-organic compounds, Sc, Zn, Ga and Ag cause the most serious interference; for organic compounds the method is rapid, and specific for fluorine.     

Determination of total fluorine in five coal reference materials by proton-induced gamma-ray emission spectrometry

The direct non-destructive proton-induced gamma-ray emission (PIGE) technique with a germanium detector was applied to the determination of total fluorine concentration in five coal reference materials (BCR 40, NIST 1632b, NIST 1635, SARM 20 and USGS CLB-1). Duplicate analyses were made from five randomly selected bottles of each coal. Individual data are presented and some problems (calibration, proton stopping power, effects of sample heating by the proton beam, background estimation) which were encountered during this study are discussed. Sensitivity and reproducibility of the determinations, and homogeneity of the coal samples with respect to fluorine contents by analysis of variance were investigated. The present data are also compared with the few published values for these reference samples, including other PIGE data. The use of synthetic standards and spiked samples in the present study suggested that the PIGE method was more accurate than other techniques.     

Proton-induced prompt gamma-ray emission for determination of light elements in human bone

Proton-induced prompt gamma-ray emission (PIGE) analysis has been used for the determination of light elements in human dense bone samples. Li, B, N, O, F, Na, Mg, Al, P and Ca peaks were detected. Smoothed, freeze-dried samples were irradiated in vacuo by 2.4 MeV protons and the induced prompt gamma rays recorded with a 110 cm³ Ge(Li) detector. Absolute concentrations were calculated on the basis of both calibration standards and pure element gamma-ray yields. The mean (±1 S. D.) concentrations as ppm or weight % obtained for 15 dense bone samples were: B 8.0 (3.3)ppm, N 12.2 (0.8)%, O 34.8 (2.3)%, F 639 (417)ppm, Na 5763 (371)ppm, Mg 2078 (290)ppm, P 9.26 (0.50)% and Ca 20.4 (1.3)%. The detection limits obtained without any prior concentration of the bone samples were: 0.3 ppm for Li, 2.0 ppm for B, 1.0% for N, 1.0% for O, 1.0 ppm for F, 3.0 ppm for Na, 50 ppm for Mg, 22 ppm for Al, 600 ppm for P and 0.8% for Ca. Detection limits for other light elements (4≤Z≤21) have also been estimated.     

Spectrographic determination of barium and strontium in geological samples

Ohne Zusammenfassung

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Polarographic determination of Tergitol 08

     

Radium determination in soil samples using a gamma-ray coincidence spectrometer

A technique for the assay of radium by detection of coincident γ-radiation is evaluated. The sensitivity of various counting modalities is compared. The influence of finite sample size and density is discussed. Interference from other natural radioactivities is investigated and it is shown that a two channel arrangement is sufficient to take this into account.     

Development of a non-destructive isotopic analysis method by gamma-ray emission measurement after negative muon irradiation

Journal of Radioanalytical and Nuclear Chemistry - Variations in isotopic abundance provide useful information for various scientific fields. Herein we performed a feasibility study by...     

Rapid non-destructive determination of thin films of platinum by particle back-scattering

Rutherford back-scattering of α-particles is used to determine trace amounts of thin films of platinum. The method is sensitive to 0.3 ng of platinum and the response is linear from at least 0.01 to 80 μg Pt cm^-2 of substrate surface area. Calibration with weighed standards reveals good accuracy and precision throughout the linear range. Up to at least 80 μg cm^-2, no matrix effects can be observed for platinum determinations on Mylar, carbon, glass, and glass or quartz coated with up to 0.5 μm thicknesses of tin oxide. Particle-induced x-ray emission spectra are included to show their utility in surface composition analysis. The analytical procedure for the determination of platinum is rapid and non-destructive, and requires minimal sample preparation.     

Rapid determination of fluorine in coral skeletons by non-destructive neutron activation analysis using 20F

A rapid non-destructive technique has been proposed for the determination of fluorine in coral skeletons by thermal neutron activation analysis, using the short half-life ²⁰F nuclide (11.0 s). About 0.2-0.5 g samples were irradiated for 10 seconds in a Triga Mark II Reactor. Soon after the irradiation (25-35 s), measurements of -rays were performed with each sample and standard. The method has the drawback of low sensitivity (20 ppm of F), and the manual operation employed in the cooling step could lead to less precise measurements. We determined fluorine in coral standards within ~8% of analytical precision. The result obtained for the dolomite standard was fairly consistent with literature values, but those for the limestone standard showed to be considerably higher than the reported values. The present method was applied for the determination of fluorine in modern corals from Khang Khao Island, Thailand and Okinawa, Japan. Two core samples of an ancient reef from Funafuti Atoll were measured for fluorine to compare with modern samples. In order to understand the environmental media in which coral grew, the partition of fluorine between seawater and coral skeletons is also discussed.     

Trace element determination in tomato puree using particle induced X-ray emission and Rutherford backscattering

Particle induced X-ray emission (PIXE) and Rutherford backscattering spectrometry (RBS) were used to determine the concentrations of trace elements in samples of 12 tomato puree brands sold in the Mexican market. While RBS offered information about the main elements present in the matrix, PIXE gave results on trace elements. As a whole, data for 17 elements (C, N, O, Na, Mg, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, and Zn) were obtained. To evaluate the results, a comparison with brands from USA, Japan, Colombia, and Chile was carried out, using tomato purees produced following the domestic technology recipe. Additionally, the results were considered in the light of the Codex Alimentarius and the Mexican standard. It was found that all of the brands fall within the limits established by these standards, being of the same order of magnitude as the foreign brands. This revised version was published online in July 2006 with corrections to the Cover Date.     

Fluorine determination in human and animal bones by particle-induced gamma-ray emission

Fluorine was determined in the iliac crest bones of patients and in ribs collected from post-mortem investigations by particle-induced gamma-ray emission based on the 19F(p,p'gamma)19F reaction, using 2.0/2.5 MeV protons. The results indicate that for 68% of the human samples the F concentration is in the range 500-1999 microg g(-1). For comparison purposes fluorine was also determined in some animal bones; in some animal tissues lateral profiles of fluorine were measured.     

Fluorine determination in human and animal bones by particle-induced gamma-ray emission

Fluorine was determined in the iliac crest bones of patients and in ribs collected from post-mortem investigations by particle-induced gamma-ray emission based on the ¹⁹F(p,p′γ)¹⁹F reaction, using 2.0/2.5 MeV protons. The results indicate that for 68% of the human samples the F concentration is in the range 500–1999 μg g^–1. For comparison purposes fluorine was also determined in some animal bones; in some animal tissues lateral profiles of fluorine were measured.     

The determination of fluorine in bones by non-destructive neutron activation analysis using 11.2 sec20F

A fast non-destructive determination of fluorine in bone samples by thermal neutron activation analysis using¹⁹F(n, γ)²⁰F reaction was developed. About 0.1–1 g samples is irradiated for 15 sec in TRIGA MARK II reactor at a thermal neutron flux of 5·10¹¹ n·cm⁻²·sec⁻¹. After 15–25 sec cooling, the 1633 KeV²⁰F activity (T=11.2 sec) is counted for 15 sec with a Ge(Li) spectrometer. A standard sample is prepared by mixing CaF₂ and CaCO₃ powders. The interference from²³Na(n, α)²⁰F is corrected by employing²⁴Na 2754 KeV double escape peak activities in samples and the²⁰F/²⁴Na peak area ratio observed previously for pure Na₂CO₃ powder. The precision is 7% for a bone sample containing 1020 ppm F and the sensitivity is about 10 ppm F.