caa a22 4500 605465606 CHVBK 20210128100303.0 cr unu---uuuuu 210128e20151201xx s 000 0 eng 10.1007/s00769-015-1161-0 doi (NATIONALLICENCE)springer-10.1007/s00769-015-1161-0 Overcoming constraints of the control charting approach for measurement uncertainty assessments [Elektronische Daten] [Amaury Borges-Miranda, Isabel Marquez-Leyva, Carlos Pérez-Martínez, Juan Jiménez-Chacón, Manuel Álvarez-Prieto] This report proposes an alternative approach for measurement uncertainty estimation avoiding the two main limitations of the control charting approach in a context were certified reference materials are unavailable. The procedures under study estimated the mass fraction of total alkaloids as nicotine and Kjeldahl total nitrogen in powdered samples of air-cured leaves of Cuban cigar tobacco. The intermediate precision estimated from results of different analysts was evaluated in parallel at three levels of mass fraction trough a spiking experiment using test portions of a one composite non-certified reference material per procedure and a balanced fully nested design. The systematic effect component was estimated in the same mass fraction levels but using a different set of samples covering a wide range of the typical routine test materials. An iterative re-weighted least squares linear regression analysis was performed between the results obtained through the assessed procedure with those attained from a reference one which analyses the same measurand. The estimation was then carried out using a proposed mathematic expression derived from the application of the uncertainty propagation law to the equation for bias estimation for every reference concentration. The uncertainty associated with bias estimation was furthermore evaluated over the whole mass fraction range considered in the procedure comparison study. The interpretation of the evaluated parameters is discussed regarding the specifics analytical characteristics of each procedure. Springer-Verlag Berlin Heidelberg, 2015 Measurement uncertainty nationallicence Non-certified reference materials nationallicence Spiking experiment nationallicence Iterative re-weighted least squares linear regression analysis nationallicence Validation nationallicence w obs : Observed mass fraction of the analyte (from the assessed procedure) represented in the ordinate (y) axis nationallicence w ref : Reference mass fraction of the analyte represented in the abscissa (x) axis nationallicence δ : Estimated bias nationallicence u 2( a ) : Variance of the intercept nationallicence u 2( b ) : Variance of the slope nationallicence u ( w ref, i ) : Uncertainty of the ith reference value nationallicence u 2( w obs, i ) : Variance of the ith data obtained by the assessed procedure nationallicence $$\bar{w}_{{{\text{ref}},i}}$$ w ¯ ref , i : Mean of the ith reference value nationallicence u c : Combined standard uncertainty nationallicence u ( δ ) : Uncertainty of the bias estimation nationallicence u c /w obs : Relative combined standard uncertainty nationallicence U : Expanded uncertainty (k=2) nationallicence U/w obs : Relative expanded uncertainty (k=2) nationallicence s ta : Standard deviation under intermediate precision estimated from results obtained at different times by different analysts nationallicence a : Intercept of a linear regression equation nationallicence b : Slope of a linear regression equation nationallicence W i : Weight for the ith data point nationallicence n : Number of measurements nationallicence Borges-Miranda Amaury Tobacco Research Institute, Carretera Tumbadero km 8 ½, San Antonio de los Baños, Artemisa, Cuba aut Marquez-Leyva Isabel Tobacco Research Institute, Carretera Tumbadero km 8 ½, San Antonio de los Baños, Artemisa, Cuba aut Pérez-Martínez Carlos Faculty of Chemistry, University of Havana, Zapata y G, Vedado, Havana, Cuba aut Jiménez-Chacón Juan Institute of Science and Technology of Materials, University of Havana, Zapata y G, s/n, Plaza, Havana, Cuba aut Álvarez-Prieto Manuel Faculty of Chemistry, University of Havana, Zapata y G, Vedado, Havana, Cuba aut Accreditation and Quality Assurance Springer Berlin Heidelberg 20/6(2015-12-01), 473-482 0949-1775 20:6<473 2015 20 769 https://doi.org/10.1007/s00769-015-1161-0 text/html Onlinezugriff via DOI BK010053 XK010053 XK010000 Metadata rights reserved Springer special CC-BY-NC licence nationallicence 1 research-article jats NATIONALLICENCE NATIONALLICENCE NL-springer NATIONALLICENCE 856 40 https://doi.org/10.1007/s00769-015-1161-0 text/html Onlinezugriff via DOI NATIONALLICENCE 700 1- Borges-Miranda Amaury Tobacco Research Institute, Carretera Tumbadero km 8 ½, San Antonio de los Baños, Artemisa, Cuba aut NATIONALLICENCE 700 1- Marquez-Leyva Isabel Tobacco Research Institute, Carretera Tumbadero km 8 ½, San Antonio de los Baños, Artemisa, Cuba aut NATIONALLICENCE 700 1- Pérez-Martínez Carlos Faculty of Chemistry, University of Havana, Zapata y G, Vedado, Havana, Cuba aut NATIONALLICENCE 700 1- Jiménez-Chacón Juan Institute of Science and Technology of Materials, University of Havana, Zapata y G, s/n, Plaza, Havana, Cuba aut NATIONALLICENCE 700 1- Álvarez-Prieto Manuel Faculty of Chemistry, University of Havana, Zapata y G, Vedado, Havana, Cuba aut NATIONALLICENCE 773 0- Accreditation and Quality Assurance Springer Berlin Heidelberg 20/6(2015-12-01), 473-482 0949-1775 20:6<473 2015 20 769