Determination Of The Content Of Hf In Zirconium Alloys With Using A Wide Band X-Ray Emission Filter

2018 ◽  
pp. 153-159
Author(s):  
O.P. Omelnyk ◽  
V.V. Levenets ◽  
A.Yu. Lonin ◽  
I.V. Shevchenko ◽  
A.O. Shchur
Keyword(s):  
Pyrolytic Graphite ◽  
Zirconium Alloys ◽  
Analytical Signal ◽  
Wide Band ◽  
Optimal Conditions ◽  
Experimental Conditions ◽  
X Ray ◽  
Method Of Determination ◽  
Non Destructive

The possibilities of a non-destructive method of determination of the content of hafnium in zirconium alloys are studied. The method is based on excitation of the characteristic X-ray emission of the atoms of the object of interest, including the L-series of atom of Hf, by external beam of protons accelerated up to 2 MeV. The excited emission is modified by a wide band X-ray emission filter, which is made from pyrolytic graphite plates and measured by a Si-PIN detector. Optimal conditions for measurement of analytical signal were determined after experimental studying. It was shown that under the selected experimental conditions and the measurement time of 10 minutes, the detection limit of Hf in the zirconium matrix is equal 20 ppm. The ways for improving of the metrological characteristics of the technique in the presence of interfering elements are proposed. The content of hafnium and uniformity of its distribution in the cladding of nuclear fuel rod made from the alloy Zr1% Nb was determined.

Development of a method for multielemental determination in water by EDXRF with radioisotopic source of 238Pu.

2019 ◽  
Vol 7 (2A) ◽  
Author(s):  
Camilo Fuentes Serrano ◽  
Juan Reinaldo Estevez Alvares ◽  
Alfredo Montero Alvarez ◽  
Ivan Pupo Gonzales ◽  
Zahily Herrero Fernandez ◽  
...  
Keyword(s):  
Thin Layer ◽  
Expanded Uncertainty ◽  
Considerable Decrease ◽  
X Ray ◽  
Precipitation Efficiency ◽  
Method Of Determination ◽  
Sensitivity Curves ◽  
Order Of Magnitude ◽  
Metrological Parameters

A method for determination of Cr, Fe, Co, Ni, Cu, Zn, Hg and Pb in waters by Energy Dispersive X Ray Fluorescence (EDXRF) was implemented, using a radioisotopic source of 238Pu. For previous concentration was employed a procedure including a coprecipitation step with ammonium pyrrolidinedithiocarbamate (APDC) as quelant agent, the separation of the phases by filtration, the measurement of filter by EDXRF and quantification by a thin layer absolute method. Sensitivity curves for K and L lines were obtained respectively. The sensitivity for most elements was greater by an order of magnitude in the case of measurement with a source of 238Pu instead of 109Cd, which means a considerable decrease in measurement times. The influence of the concentration in the precipitation efficiency was evaluated for each element. In all cases the recoveries are close to 100%, for this reason it can be affirmed that the method of determination of the studied elements is quantitative. Metrological parameters of the method such as trueness, precision, detection limit and uncertainty were calculated. A procedure to calculate the uncertainty of the method was elaborated; the most significant source of uncertainty for the thin layer EDXRF method is associated with the determination of instrumental sensitivities. The error associated with the determination, expressed as expanded uncertainty (in %), varied from 15.4% for low element concentrations (2.5-5 μg/L) to 5.4% for the higher concentration range (20-25 μg/L).

Stoichiometric Determination of Graphite Intercalation Compounds Using Rutherford Backscatiering Spectrometry

1983 ◽  
Vol 27 ◽  
Author(s):  
L. Salamanca-Riba ◽  
B.S. Elman ◽  
M.S. Dresselhaus ◽  
T. Venkatesan
Keyword(s):  
Experimental Error ◽  
Rutherford Backscattering Spectrometry ◽  
Rutherford Backscattering ◽  
Intercalation Compounds ◽  
Graphite Intercalation Compounds ◽  
X Ray ◽  
Donor And Acceptor ◽  
Graphite Intercalation ◽  
Non Destructive

ABSTRACTRutherford backscattering spectrometry (RBS) is used to characterize the stoichiometry of graphite intercalation compounds (GIC). Specific application is made to several stages of different donor and acceptor compounds and to commensurate and incommensurate intercalants. A deviation from the theoretical stoichiometry is measured for most of the compounds using this non-destructive method. Within experimental error, the RBS results agree with those obtained from analysis of the (00ℓ) x-ray diffractograms and weight uptake measurements on the same samples.

ANALYSIS OF SOLDERS ON TIN AND LEAD BASES BY X-RAY FLOORESCENT SPECTROSCOPY

2021 ◽  
pp. 124-131
Author(s):  
A.V. Alekseev ◽  
◽  
G.V. Orlov ◽  
P.S. Petrov ◽  
A.V. Slavin ◽  
...  
Keyword(s):  
Emission Spectroscopy ◽  
High Resolution Mass Spectrometry ◽  
Analytical Signal ◽  
Atomic Emission ◽  
Standard Samples ◽  
X Ray ◽  
Fundamental Parameters ◽  
The Matrix ◽  
Resolution Mass

The determination of the elements Cu, Ni, Sb, Bi, Pb, Zn and Fe in the tin-based solder VPr35, as well as the elements Sn, Ni, Sb, Bi and In in the lead-based VPr40 solder by the method of х-ray fluorescence spectroscopy has been carried out. The calibration dependences are corrected taking into account the superposition of signals from interfering elements on the analytical signal and changes in intensity caused by inter-element influences in the matrix. The analysis was carried out by the method of fundamental parameters without using standard samples. The correctness of the results obtained was confirmed by their comparative analysis by atomic emission spectroscopy and high-resolution mass spectrometry with a glow discharge.

A Two-step Electrodeposition of Pd-Cu/Cu2O Nanocomposite on FTO Substrate for Non-enzymatic Hydrogen Peroxide Sensor

2021 ◽  
Vol 17 ◽  
Author(s):  
Ke Huan ◽  
Li Tang ◽  
Dongmei Deng ◽  
Huan Wang ◽  
Xiaojing Si ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
Cyclic Voltammetry ◽  
Photoelectron Spectroscopy ◽  
Chemical Structure ◽  
Pd Nanoparticles ◽  
Optimal Conditions ◽  
Potential Oscillation ◽  
X Ray Diffraction ◽  
X Ray

Background: Hydrogen peroxide (H2O2) is a common reagent in the production and living, but excessive H2O2 may enhance the danger to the human body. Consequently, it is very important to develop economical, fast and accurate techniques for detecting H2O2. Methods: A simple two-step electrodeposition process was applied to synthesize Pd-Cu/Cu2O nanocomposite for non-enzymatic H2O2 sensor. Cu/Cu2O nanomaterial was firstly electrodeposited on FTO by potential oscillation technique, and then Pd nanoparticles were electrodeposited on Cu/Cu2O nanomaterial by cyclic voltammetry. The chemical structure, component, and morphology of the synthesized Pd-Cu/Cu2O nanocomposite were characterized by X-ray diffraction, scanning electron microscopy and X-ray photoelectron spectroscopy. The electrochemical properties of Pd-Cu/Cu2O nanocomposite were studied by cyclic voltammetry and amperometry. Results: Under optimal conditions, the as-fabricated sensor displayed a broad linear range (5-4000 µM) and low detection limit (1.8 µM) for the determination of H2O2. The proposed sensor showed good selectivity and reproducibility. Meanwhile, the proposed sensor has been successfully applied to detect H2O2 in milk. Conclusion: The Pd-Cu/Cu2O/FTO biosensor exhibits excellent electrochemical activity for H2O2 reduction, which has great potential application in the field of food safety.

Determination of the Hydrogen Concentration in Zr-2.5Nb Alloy by a Resonant Ultrasound Spectroscopy

2006 ◽  
Vol 321-323 ◽  
pp. 1576-1579
Author(s):  
Yong Moo Cheong ◽  
Young Suk Kim
Keyword(s):  
Hydrogen Concentration ◽  
Zirconium Alloy ◽  
Nuclear Reactor ◽  
Zirconium Alloys ◽  
Resonant Ultrasound Spectroscopy ◽  
Heavy Water Reactor ◽  
Resonant Ultrasound ◽  
Non Destructive

Zirconium alloys are used for many applications in nuclear components, such as the pressure tube material in a pressurized heavy water reactor, nuclear fuel cladding, etc. One of the problems during the operation of a nuclear reactor is the degradation of the zirconium alloys, which is due to an increase of the hydrogen content in the zirconium alloy. Therefore a non-destructive determination of the hydrogen concentration in zirconium alloy is one of the important issues that need to be addressed. The resonant ultrasound spectroscopy (RUS) technique is evaluated for a characterization of the hydrogen concentration in Zr-2.5Nb alloy. Referring to the terminal solid solubility for dissolution (TSSD) of Zr-2.5Nb alloy, the plot of the mechanical damping coefficient (Q-1) versus the temperature or the deviation of the resonant frequency for the temperature (df/dT) versus the temperature was correlated for the hydrogen concentration in Zr-2.5Nb alloy. It was found that the temperature at an abrupt change of the slope can be correlated with the hydrogen concentration of the Zr-2.5Nb alloy.

scholarly journals APPLICATION OF MATHEMATICAL PLANNING OF THE EXPERIMENT IN THE CHOOSING THE OPTIMUM CONDITIONS OF THE VAPOR-PHASE GAS-CHROMATOGRAPHIC DETERMINATION OF FORMALDEHYDE IN THE URINE

2018 ◽  
Vol 97 (10) ◽  
pp. 985-989 ◽  
Author(s):  
Аnton N. Alekseenko ◽  
O. M. Zhurba
Keyword(s):  
Mathematical Model ◽  
Vapor Phase ◽  
Statistical Processing ◽  
Analytical Signal ◽  
Heating Time ◽  
Gas Extraction ◽  
Optimal Conditions ◽  
Steep Ascent ◽  
The Mathematical Model

Introduction. There was substantiated a method for the determination of formaldehyde by vapor-phase gas chromatography by the use of derivatizing reagent o-(2,3,4,5,6-pentafluorbenzyl)hydroxylamine. Material and methods. Formaldehyde in urine was derivatized to o-pentafluorobenzyloxime and recovered to the vapor phase by heating the urine sample with o-(2,3,4,5,6-pentafluorbenzyl)hydroxylamine in a sealed vial. Gas-chromatographic analysis of the vapor-air phase was performed in a mode of the temperature gradient on a capillary column HP-5 with a flame ionization detector. Identification of the analyte in the form of the derivative-o- pentafluorobenzyloxime of formaldehyde was carried out according to the absolute retention time, which was established by comparing the chromatograms of model formaldehyde mixtures in the urine of different concentrations. Results. The optimal conditions for gas extraction are selected using mathematical experimental planning. The most important factors of gas extraction in the vapor-phase analysis are the temperature and time of the establishment of the interphase equilibrium with heating. From the experimentally obtained curves of the analytical signal on the temperature and the heating time, the zero level and the interval of variation of these factors are chosen. A matrix for planning a 2-factor experiment was constructed. The coefficients of the mathematical model are determined. There was carried out statistical processing of the experimental data, which was reduced to the estimation of the reproducibility of the optimization parameter and to the evaluation of the significance of the coefficient of the mathematical model. The adequacy of the mathematical model was evaluated, its interpretation was carried out. Discussion. The peak area of the analyte increases with the elevating the temperature and heating time, due to an increase in the analyte concentration in the vapor phase. Moreover, the heating time makes a greater contribution to the formation of the analytical signal than the temperature. The step of motion along the gradient was calculated and the experiments of steep ascent were carried out. Conclusion. According to the results of the steep ascent experiments, the optimal conditions for the gas extraction of formaldehyde in the form of a derivative were chosen.

Standardisation of X-Ray Powder Diffraction Methods

2004 ◽  
Vol 443-444 ◽  
pp. 31-34
Author(s):  
Giovanni Berti ◽  
Rob Delhez ◽  
S. Norval ◽  
B. Peplinski ◽  
E. Tolle ◽  
...  
Keyword(s):  
Technical Committee ◽  
Non Destructive Testing ◽  
X Ray Diffraction ◽  
Destructive Testing ◽  
X Ray ◽  
Standard Documents ◽  
And Control ◽  
Non Destructive ◽  
Research Centres

This paper outlines the standardisation process for the XRPD method that is currently being considered by a Working Group (WG10) of Technical Committee 138 "Non-destructive Testing" of the European Committee for Standardisation CEN. Several Standard Documents are on the verge of being released. These documents concern the general principles of (X-ray) diffraction, its terminology, and the basic procedures applied. Another document concerns the instruments used and it offers procedures to characterise and control the performance of an X-ray diffractometer properly. It is intended to issue Standard Documents on specific methods, e.g. determination of residual stresses. In fact work is in progress on this subject. The Standard Documents can be used by industry, government organisations, and research centres with activities related to safety, health and the environment, as well as for educational purposes.

X-ray topographic determination of the granular structure in a graphite mosaic crystal: a three-dimensional reconstruction

2000 ◽  
Vol 33 (4) ◽  
pp. 1023-1030 ◽  
Author(s):  
M. Ohler ◽  
M. Sanchez del Rio ◽  
A. Tuffanelli ◽  
M. Gambaccini ◽  
A. Taibi ◽  
...  
Keyword(s):  
Structural Parameters ◽  
Pyrolytic Graphite ◽  
Three Dimensional ◽  
X Ray ◽  
Dimensional Reconstruction ◽  
Mosaic Crystals ◽  
Spatial Locations ◽  
Crystalline Domains

Section topographs recorded at different spatial locations and at different rocking angles of a highly oriented pyrolytic graphite (HOPG) crystal allow three-dimensional maps of the local angular-dependent scattering power to be obtained. This is performed with a direct reconstruction from the intensity distribution on such topographs. The maps allow the extraction of information on local structural parameters such as size, form and internal mosaic spread of crystalline domains. This data analysis leads to a new method for the characterization of mosaic crystals. Perspectives and limits of applicability of this method are discussed.

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