Limit of detection for second-order calibration methods
MARÍA JOSÉ RODRÍGUEZ CUESTA Doctoral Thesis ROVIRA I VIRGILI UNIVERSITY Tarragona 2006
Table of contents Chapter 1. DESCRIPTION OF THE THESIS 1.1. Motivation ................................................................................... -3- 1.2. Objectives .................................................................................... -4- 1.3. Structure ..................................................................................... -6- 1.4. Notation and list of symbols ...................................................... -8-
Chapter 2. INTRODUCTION TO CHEMOMETRICS 2.1. Types of data and instruments used in Analytical Chemistry-13- 2.1.1. Historical Background........................................................................-13- 2.1.2. Tensor Terminology...........................................................................-14- 2.1.3. The Concepts of Bilinearity and Trilinearity .......................................-17- 2.1.4. Deviations from Linearity ...................................................................-20-
2.2. Calibration methods.................................................................... -22- 2.2.1. From Zeroth- to Second-order Calibration.........................................-22- 2.2.2. Resolution and Calibration Methods for Second-Order Data.............-27- 2.2.2.1 Parallel Factor Analysis (PARAFAC) ...................................-31- 2.2.2.2 Iterative Target Transformation Factor Analysis (ITTFA).....-35- 2.2.2.3 Multivariate Curve Resolution-Alternating Least Squares (MCR-ALS) ..........................................................................-38- 2.2.2.4 Multi-linear Partial Least Squares (N-PLS) ..........................-41- 2.2.3. Uniqueness, Indeterminacies and Constraints ..................................-44-
2.3. Validation of Analytical Methods .............................................. -50- 2.3.1. What is Method Validation? ..............................................................-50- 2.3.2. Figures of Merit. International Recommendations .............................-51- 2.3.3. Analytical Detection ......................................................................... -55- 2.3.3.1 Hypothesis Testing ............................................................ -55- 2.3.3.2 Critical Level and Detection Limit ...................................... -56- 2.3.3.3 Limit of Detection from Linear Calibration Curves............... -58- 2.3.3.4 Limit of Detection in Multivariate Calibration ....................... -61- ter 3. ESTIMATION OF THE LOD FOR PARAFAC 3.1. Introduction..................................................................................-69- 3.2. Paper.............................................................................................-73- Determination of Carbendazim, Fuberidazole and Thiabendazole by Three- Dimensional Excitation–Emission Matrix Fluorescence and Parallel Factor Analysis. Analytica Chimica Acta 491: 47-57 (2003) Chapter 4. ESTIMATION OF THE LOD FOR ITTFA 4.1. Introduction..................................................................................-95- 4.2. Paper.............................................................................................-99- Influence of Selectivity and Sensitivity Parameters on Detection in Multivariate Curve Resolution of Chromatographic Second-Order Data. Analytica Chimica Acta 476: 111-122 (2003)
Chapter 5. ESTIMATION OF THE LOD FOR MCR-ALS 5.1. Introduction..................................................................................-125- 5.2. Paper.............................................................................................-129- Development and Validation of a Method for Determining Pesticides in Groundwater from Complex Overlapped HPLC Signals and Multivariate Curve Resolution. Chemometrics and Intelligent Laboratory Systems 77(1- 2): 251-260 (2005) Chapter 6. ESTIMATION OF THE LOD FOR N-PLS 6.1. Introduction ................................................................................. -157- 6.2. Paper............................................................................................. -161- Standard Error of Prediction at Low Content Levels and Limit of Detection Estimation for Multivariate and Multi-linear Regression. (In press)
APPENDIX References ........................................................................................... -201- Glossary and abbreviations.................................................................. -211- List of papers and meeting contributions ............................................. -221- Limit of detection for second-order calibration methods
Limit of detection for second-order calibration methods
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