Laura Giordani

The detection of signals hidden in noise

This paper examines signal detection in the presence of noise, with particular emphasis on nuclear activation analysis. The specific problem is to decide whether the signal-plus-background or the no-signal hypothesis fits the data better. Our solution is based on the use of Bayesian inferences to test the two hypotheses.

Neutron activation analysis of the 30Si content of highly enriched 28Si: proof of concept and estimation of the achievable uncertainty

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 modelled 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.

Use of Instrumental Neutron Activation Analysis to investigate the distribution of trace elements among subsamples of solid materials

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 the 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.

Report of the key comparison CCQM-K108 determination of arsenic species, total arsenic and cadmium in brown rice flour

The CCQM-K108 key comparison was organised by the Inorganic Analysis Working Group (IAWG) of CCQM to test the abilities of national metrology institutes (NMIs) or designated institutes (DIs) to measure the mass fractions of arsenic species, total arsenic and cadmium in brown rice flour. The National Metrology Institute of Japan (NMIJ) acted as the coordinating laboratory. The participants used different measurement methods, though most of them used inductively coupled plasma mass spectrometry (ICP-MS) or isotope-dilution inductively coupled plasma mass spectrometry (ID-ICP-MS) for Cd and ICP-MS for total arsenic. Regarding arsenic speciation, all participants used ICP-MS coupled with liquid chromatography (LC). Accounting for relative expanded uncertainty, comparability of measurement results for each of total arsenic and cadmium was successfully demonstrated by the participating NMIs or DIs for the measurement of the measurand at the level of less than 0.5 mg/kg. Regarding arsenic species (inorganic arsenic and dimethylarsinic acid (DMAA)), there was, however, a measurement problem still to be solved and that part of CCQM-K108 will be repeated. It is expected that arsenic, cadmium and other metals at mass fractions greater than approximately 0.1 mg/kg in rice flour can be determined by each participant using the same technique(s) employed for this key comparison to achieve similar uncertainties mentioned in the present report. Furthermore, the results of this key comparison can be utilised along with the IAWG core capability approach. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).