Issue 7, 2002

Worst case uncertainty estimates for routine instrumental analysis

Abstract

A methodology for the worst case measurement uncertainty estimation for analytical methods which include an instrumental quantification step, adequate for routine determinations, is presented. Although the methodology presented should be based on a careful evaluation of the analytical method, the resulting daily calculations are very simple. The methodology is based on the estimation of the maximum value for the different sources of uncertainty and requires the definition of limiting values for certain analytical parameters. The simplification of the instrumental quantification uncertainty estimation involves the use of the standard deviation obtained from control charts relating to the concentrations estimated from the calibration curves for control standards at the highest calibration level. Three levels of simplification are suggested, as alternatives to the detailed approach, which can be selected according to the proximity of the sample results to decision limits. These approaches were applied to the determination of pesticide residues in apples (CEN, EN 12393), for which the most simplified approach showed a relative expanded uncertainty of 37.2% for a confidence level of approximately 95%.

Article information

Article type
Paper
Submitted
02 Feb 2002
Accepted
26 Apr 2002
First published
07 Jun 2002

Analyst, 2002,127, 957-963

Worst case uncertainty estimates for routine instrumental analysis

R. J. N. Bettencourt da Silva, J. R. Santos and M. F. G. F. C. Camões, Analyst, 2002, 127, 957 DOI: 10.1039/B201362M

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