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Register a new userInstrumental neutron activation analysis of an enriched 28Si single-crystal
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Added by
Giancarlo D'Agostino Dr.
Publication date
2013
fields
Physics
and research's language is
English
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The determination of the Avogadro constant plays a key role in the redefinition of the kilogram in terms of a fundamental constant. The present experiment makes use of a silicon single-crystal highly enriched in 28Si that must have a total impurity mass fraction smaller than a few parts in 109. To verify this requirement, we previously developed a relative analytical method based on neutron activation for the elemental characterization of a sample of the precursor natural silicon crystal WASO 04. The method is now extended to fifty-nine elements and applied to a monoisotopic 28Si single-crystal that was grown to test the achievable enrichment. Since this crystal was likely contaminated, this measurement tested also the detection capabilities of the analysis. The results quantified contaminations by Ge, Ga, As, Tm, Lu, Ta, W and Ir and, for a number of the detectable elements, demonstrated that we can already reach the targeted 1 ng/g detection limit.
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We investigated the use of neutron activation to estimate the 30Si mole fraction of the ultra-pure silicon material highly enriched in 28Si for the measurement of the Avogadro constant. Specifically, we developed a relative method based on Instrumental Neutron Activation Analysis and using a natural-Si sample as a standard. To evaluate the achievable uncertainty, we irradiated a 6 g sample of a natural-Si material and modeled experimentally the signal that would be produced by a sample of the 28Si-enriched material of similar mass and subjected to the same measurement conditions. The extrapolation of the expected uncertainty from the experimental data indicates that a measurement of the 30Si mole fraction of the 28Si-enriched material might reach a 4% relative combined standard uncertainty.
The results of analytical measurements performed with solid-sampling techniques are affected by the distribution of the analytes within the matrix. The effect becomes significant in case of determination of trace elements in small subsamples. In this framework we propose a measurement model based on Instrumental Neutron Activation Analysis to determine the relative variability of the amount of an analyte among subsamples of a material. The measurement uncertainty is evaluated and includes the counting statistics, the full-energy gamma peak efficiency and the spatial gradient of the neutron flux at the irradiation position. The data we obtained in a neutron activation experiment and showing the relative variability of As, Au, Ir, Sb and W among subsamples of a highly pure Rh foil are also presented.
The latest determination of the Avogadro constant, carried out by counting the atoms in a pure silicon crystal highly enriched in 28Si, reached the target 2x10-8 relative uncertainty required for the redefinition of the kilogram based on the Planck constant. The knowledge of the isotopic composition of the enriched silicon material is central; it is measured by isotope dilution mass spectrometry. In this work, an independent estimate of the 30Si mole fraction was obtained by applying a relative measurement protocol based on Instrumental Neutron Activation Analysis. The amount of 30Si isotope was determined by counting the 1266.1 keV gamma-photons emitted during the radioactive decay of the radioisotope 31Si produced via the neutron capture reaction 30Si(n,gamma)31Si. The x(30Si) = 1.043(19)x10-6 mol mol-1 is consistent with the value currently adopted by the International Avogadro Coordination.
An instrument and software algorithm is described for the purpose of characterization of large single crystals at the Alignment Facility (ALF) of the ISIS spallation neutron source. We describe a method for both characterizing the quality of the sample and also aligning it in a particular scattering plane. We present a software package written for this instrument and demonstrate its utility by way of an example of the structural characterization of large singles crystals of Pb(Mg$_{1/3}$Nb$_{2/3}$)O$_{3}$. We suggest extensions and modifications of characterization instruments for future improved beamlines. It is hoped that this software will be used by the neutron user community for pre characterizing large single crystals for spectroscopy experiments and that future facilities will include such a facility as part of the spectroscopy suite at spallation neutron sources.
Features of forward diffracted Parametric X-Radiation (PXR) were investigated at experiments with the 855 MeV electron beam of the Mainz Microtron MAMI employing a 410 micrometer thick tungsten single crystal. Virtual photons from the electron field are diffracted by the (10-1) plane at a Bragg angle of 3.977 degree. Forward emitted radiation was analyzed at an energy of 40 keV with the (111) lattice planes of a flat silicon single crystal in Bragg geometry. Clear peak structures were observed in an angular scan of the tungsten single crystal. The results were analyzed with a model which describes forward diffracted PXR under real experimental conditions. The experiments show that forward diffracted PXR may be employed to diagnose bending radii of lattice planes in large area single crystals.
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