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- 2014 (2) (entfernen)
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- Calibration samples (1)
- Electrical parameters (1)
- Fast flow source (1)
- Glow discharge mass spectrometry (1)
- Homogeneity (1)
- Instrumental neutron activation analysis (1)
- Magnesium matrix (1)
- Non-metals (1)
- Nonmetallic impurities (1)
- Powders (1)
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.
Fast flow glow discharge mass spectrometry with a Grimm-type ion source providing a high sputter rate was used for the determination of major nonmetallic impurities in magnesium. The analytical signal was found to be strongly influenced by the electrical discharge parameters. For calibration by standard addition, synthetic standard samples were produced in two different ways—namely, by pressing and by sintering doped metal powders. The observed sensitivity of the calibration curves was shown to depend on the particle size of the powder. For the magnesium powders, the mass fractions of oxygen, nitrogen, boron, and silicon were determined to be about 0.01 kg·kg-1 (relative standard deviation approximately 10–20 %), 2,700 mg·kg-1, 150 mg·kg-1, and 300 mg·kg-1, respectively.