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Eingeladener Vortrag
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Analysis of natural gas by gas chromatography Reduction of correlated uncertainties by normalisation
(2004)
The results of gas chromatographic analysis of natural gas mixtures reveal strong correlations (Pearson correlation coefficient of >0.96) between the uncertainty of each component and variations in the ambient pressure. Although correction for ambient pressure variations can reduce this variability, normalisation of the results of each analysis using the assumption that the sum of all component amount fractions is unity provides significantly greater reductions in the uncertainty of each measured component. We show that the uncertainty in normalised components can be estimated approximately using the correlation coefficient as a measure of the correlation present in the measurements, or exactly using a full calculation of the variance/covariance (V/C) structure of the data.
Zusammenfassung
If the value of a derived measurement standard is assigned by comparison with a reference standard of the same quantity, the uncertainty is increased by the additional uncertainty on the difference measurement. This basic fact has lead to the general belief that the uncertainty of derived standards is always larger than that of the reference standards. However, if the value of a derived standard is assigned by comparison with several independent reference standards using an appropriate average, the increase of uncertainty due to the uncertainty on difference measurement may be counterbalanced by the the well-known decrease of uncertainty through averaging. The gain of accuracy made possible by this mechanism is restricted to second-generation standards. Further gain through iteration is prevented by correlation between standards derived from the same set of reference standards. As a consequence, the concept of metrological hierarchy levels, relating to traceability chains, becomes questionable for traceability networks.
Uncertainty propagation via preparation, calibration and comparison steps in traceability networks
(1999)
With measurement uncertainty estimation accounting for all relevant uncertainty contributions, the results of measurements using the same procedure on different objects or samples may no longer be considered as being independent, and correlations have to be taken into account. For this purpose, a simple approximation for the estimation of covariances is derived and applied to the estimation of uncertainty for some basic combinations of two measurement results. This covariance estimate is also applied to the estimation of uncertainty for the mean value of the results of replicate measurements on the same object or sample.
A first international 26Al interlaboratory comparison was initiated and evaluation of the results of the eight participating accelerator mass spectrometry (AMS) laboratories on four synthetic samples shows no difference in the sense of simple statistical significance. However, certain interlaboratory bias is observed with more detailed statistical analyses. Some laboratories seem to underestimate the uncertainties of their measurements, and others may overestimate measurement reproducibility.
KALIBRIERUNSICHERHEIT?
(2004)
After finishing Part I of the first international 26Al interlaboratory comparison with accelerator mass spectrometry (AMS) laboratories [S. Merchel, W. Bremser, Nucl. Instr. and Meth. B 223224 (2004) 393], the evaluation of Part II with radionuclide counting laboratories took place. The evaluation of the results of the seven participating laboratories on four meteorite samples shows a good overall agreement between laboratories, i.e. it does not reveal any statistically significant differences if results are compared sample-by-sample. However, certain interlaboratory bias is observed with a more detailed statistical analysis including some multivariate approaches.
Deoxynivalenol (DON), nivalenol (NIV) and zearalenone (ZEN) are toxic secondary metabolites produced by several species of Fusarium fungi. These mycotoxins are often found together in a large variety of cereal-based foods, which are regulated by maximum content levels of DON and ZEN. To date, suitable certified reference materials (CRM) intended for quality control purposes are lacking for these Fusarium mycotoxins. In order to overcome this lack, the first CRM for the determination of DON, NIV and ZEN in naturally contaminated wheat flour (ERM®-BC600) was developed in the framework of a European Reference Materials (ERM®) project. This article describes and discusses the whole process of ERM®-BC600 development, including material preparation, homogeneity and stability studies, and an interlaboratory comparison study for certification. A total of 21 selected expert laboratories from different European countries with documented expertise in the field of mycotoxin analysis took part in the certification study using various gas and liquid chromatographic methods. The certified values and their corresponding expanded uncertainties (k=2) were assigned in full compliance with the requirements of ISO Guide 35 and are as follows: 102±11 µgkg-1 for DON, 1000±130 µgkg-1 for NIV and 90±8 µgkg-1 for ZEN.