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Calibration-Free Laser-Induced Breakdown Spectroscopy (CF-LIBS) has been proposed several years ago as an approach for quantitative analysis of Laser-Induced Breakdown Spectroscopy spectra. Recently developed refinement of the spectral processing method is described in the present work. Accurate quantitative results have been demonstrated for several metallic alloys. However, the degree of accuracy that can be achieved with Calibration-Free Laser-Induced Breakdown Spectroscopy analysis of generic samples still needs to be thoroughly investigated. The authors have undertaken a systematic study of errors and biasing factors affecting the calculation in the Calibration-Free Laser-Induced Breakdown Spectroscopy spectra processing. These factors may be classified in three main groups: 1) experimental aberrations (intensity fluctuations and inaccuracy in the correction for spectral efficiency of a detection system), 2) inaccuracy in theoretical parameters used for calculations (Stark broadening coefficients and partition functions) and 3) plasma non-ideality (departure from thermal equilibrium, spatial and temporal inhomogeneities, optical thickness, etc.). In this study, the effects of experimental aberrations and accuracy of spectral data were investigated, assuming that the analytical plasma is ideal. Departure of the plasma conditions from ideality will be the object of future work. The current study was based on numerical simulation. Two kinds of metallic alloys, iron-based and aluminum-based, were studied. The relative weight of the error contributions was found to depend on the sample composition. For the here-investigated samples, the experimental aberrations contribute to the overall uncertainty on the quantitative results more than theoretical parameters. The described simulation method can be applied to the Calibration-Free Laser-Induced Breakdown Spectroscopy analysis of any other kind of sample.
Lateral resolution of secondary ion mass spectrometry - results of an inter-laboratory comparison
(2007)
Recently, BAM organised an inter-laboratory comparison focussed on lateral resolution and accuracy of sub-micron length measurements by secondary ion mass spectrometry (SIMS). Results were submitted by 16 laboratories from 10 countries. The task was to analyse a cross-sectioned semiconductor multilayer stack. The resulting strip pattern in the surface of the sample shows narrow strips, step transitions and gratings of different periods. Imaging analysis of this pattern enables the determination of relevant parameters related to the lateral resolution: (i) The width (FWHM) of the primary ion beam, (ii) the distance between 16% and 84% intensity points in a profile across the image of a step transition and (iii) the modulation of intensity in the images of gratings with different periods. The parameter's data reported by the participants vary in a wide range. A strong variation in the data of primary ion beam width was observed for results measured with the same type of instrument. The distance between two narrow strips was measured with high accuracy. Twelve of sixteen of the submitted values are within the limits of uncertainty of the reference value 964 ± 35 nm. This result shows that the calibration of the length scale of the SIMS instruments is already rather precise in most of the participating laboratories.
Data correction is probably the least favourite activity amongst users experimenting with small-angle X-ray scattering: if it is not done sufficiently well, this may become evident only during the data analysis stage, necessitating the repetition of the data corrections from scratch. A recommended comprehensive sequence of elementary data correction steps is presented here to alleviate the difficulties associated with data correction, both in the laboratory and at the synchrotron. When applied in the proposed order to the raw signals, the resulting absolute scattering cross section will provide a high degree of accuracy for a very wide range of samples, with its values accompanied by uncertainty estimates. The method can be applied without modification to any pinhole-collimated instruments with photon-counting direct-detection area detectors.
Growing awareness of the impact of monoterpenes on climate, atmospheric chemistry, and indoor air quality has necessitated the development of measurement standards to globally monitor and control their emissions. For National Metrology Institutes to develop such standards, it is essential that they demonstrate measurement equivalence for assigned values at the highest levels of accuracy. This report describes the results of a pilot comparison for 4 key monoterpene species: α-pinene, 3-carene, R-limonene and 1,8-cineole, at a nominal amount-of-substance fraction of 2.5 nmol mol-1. The objective of this comparison is to evaluate participant capabilities to measure trace-level monoterpenes using their own calibration techniques.
Thermal fluctuations do exist at extensometers but they remain quite often unknown because the temperature of the extensometer is not measured, recorded and assessed in strain controlled tests. The temperature fluctuation leads to thermal expansion of the gauge length of the extensometer resulting in force fluctuations as a materials response of the material tested in a strain controlled test. The thermal expansion leads to an error of the strain range applied.
A case study was conducted to calculate the strain range error when the strain range was varied as well as the thermal fluctuation of the extensometer. The most important outcome of the study is that the strain range error can exceed the allowed limits if the thermal fluctuation of the extensometer is too high. Sources of thermal fluctuation of the extensometer were analyzed and identified. Suggestions are given to reduce the thermal fluctuation of the extensometer.