Validation an Example extras验证一个例子.springer.pptVIP

Validation: an Example Validation Must Be Performance Based Worked Example: Fe2O3 in MgO Deriving Minimum Performance Characteristics from Requirements Preliminary Examination of Candidate Methods (1) Preliminary Examination of Candidate Methods (2) Validation Plan Calibration without MgO Calibration with MgO Graphical Comparison EXCEL Macro ValiData Numerical Comparison Limits of DetectionLimits of Quantitation Estimation of Recovery Alternative Method: Titrimetry Estimation of Uncertainty from Sampling Content of Validation Report *W. Wegscheider Validation: an Example B. Neidhart, W. Wegscheider (Eds.): Quality in Chemical Measurements ? Springer-Verlag Berlin Heidelberg 2000 * Learning Objectives: Student is able to inquire in sufficient depth on the purpose of analytical work is able to translate this information into stepwise strategy keeping in mind suitable performance characteristics at each step can devise experiments to test against these criteria performs statistical analysis of obtained data with the goal to make a valid judgement regarding the suitability of the method Definition of the need of the client translated to analytical quality criteria including cost and time Compilation of candidate methods Critical appraisal of candidate methods with respect to expected method performance Design and execution of validation study Evaluation of results, go-ahead or modifications or alternative method Measure the unknown with due regard to previously established quality criteria For certain industrial applications of MgO the upper limit of Fe oxide needs to be controlled very tightly Definition of the need of the customer translated to analytical quality criteria including cost and time In this application an upper limit of 0.5 % was guaranteed by the supplier, the customer found 0.64 %, the supplier 0.41 %. overall uncertainty (including sampling): 0.03 % uncertainty at required level of concentrationfrom analysis itself: ~0.01% limit of