Pitfalls and Errors of HPLC in Pictures / Edition 1

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Overview

Adding 13 examples to this new, third edition, Veronika Meyer now offers solutions for nearly 100 problems. All the examples are accompanied by a concise, instructive text and an informative figure, including essential fundamentals as well as such helpful strategies as equipment tests or quality assurance strategies. A practice-oriented aid to obtaining correct and reliable analytical results.

From the reviews of a previous edition:
'This is a giant of a little book on HPLC.'
(Analytical Chemistry)

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Product Details

  • ISBN-13: 9783527313723
  • Publisher: Wiley
  • Publication date: 4/28/2006
  • Edition description: 2nd, Revised and Enlarged Edition
  • Edition number: 1
  • Pages: 199
  • Product dimensions: 6.79 (w) x 9.57 (h) x 0.41 (d)

Meet the Author

Following an apprenticeship as laboratory assistant, Veronika R. Meyer studied chemistry at the university of applied sciences in Burgdorf (Switzerland). From 1976 to 1998 she worked with HPLC at Berne University, where she also completed her PhD thesis in Chemistry. Afterwards she spent her post-doc time at the Weizmann-Institute in Rehovot (Israel) and at the University of Delaware, Newark, DE. Since 1998 she is working for EMPA (Swiss Federal Laboratories for Materials Testing and Research) in St. Gallen. The fist German edition of her textbook "Practical High-Performance Liquid Chromatography" was published in 1979. Veronika R. Meyer is author of numerous papers in international journals and teaches at Berne University.

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Table of Contents

Preface.

Introduction.

Part I: Fundamentals.

1.1 Chromatography.

1.2 Chromatographic Figures of Merit.

1.3 The Resolution of Two Peaks.

1.4 Reduced Parameters.

1.5 The Van Deemter Curve.

1.6 Peak Capacity and Number of Possible Peaks.

1.7 Statistical Resolution Probability: Simulation.

1.8 Statistical Resolution Probability: Example.

1.9 Precision and Accuracy of an Analytical Result.

1.10 Standard Deviation.

1.11 Uncertainty Propagation.

1.12 Reproducibility in Trace Analysis.

1.13 Ruggedness.

1.14 Calibration Curves.

1.15 The HPLC Instrument.

1.16 The Detector Response Curve.

1.17 Noise.

1.18 Causes and Effects Presented as an Ishikawa Diagram.

1.19 The Possible and the Impossible.

Part II: Pitfalls and Sources of Error.

2.1 Mixing of the Mobile Phase.

2.2 Mobile Phase pH.

2.3 Adjustment of Mobile Phase pH.

2.4 Inadequate Purity of a Mobile Phase Solvent.

2.5 Inadequate Purity of a Mobile Phase Reagent.

2.6 System Peaks and Quantitative Analysis.

2.7 Sample Preparation with Solid Phase Extraction.

2.8 Poor Choice of Sample Solvent: Peak Distortion.

2.9 Poor Choice of Sample Solvent: Tailing.

2.10 Sample Solvent and Calibration Curve.

2.11 Impurities in the Sample.

2.12 Formation of a By-Product in the Sample Solution.

2.13 Decomposition by the Sample Vial.

2.14 Artifact Peaks from the Vial Septum.

2.15 Formation of an Associate in the Sample Solution.

2.16 Precision and Accuracy with Loop Injection.

2.17 Injection Technique.

2.18 Injection of Air.

2.19 Sample Adsorption in the Loop.

2.20 Extra-Column Volumes.

2.21 Dwell Volume.

2.22 Elution at t0.

2.23 Classification of C18 Reversed Phases.

2.24 Different Selectivity of C18 Reversed Phases.

2.25 Different Batches of Stationary Phase.

2.26 Chemical Reaction within the Column.

2.27 Recovery and Peak Shape Problems with Proteins.

2.28 Double Peaks from Stable Conformers.

2.29 Influence of Temperature on the Separation.

2.30 Thermal Non-Equilibrium within the Column.

2.31 Influence of the Volume Flow Rate on the Separation.

2.32 Influence of Run Time and Volume Flow Rate on Gradient Separations.

2.33 UV Spectra and Quantitative Analysis.

2.34 UV Detection Wavelength.

2.35 Fluorescence Quenching by Air.

2.36 Detector Overload.

2.37 Influence of the Retention Factor on Peak Height.

2.38 Influence of the Volume Flow Rate on Peak Area.

2.39 Leaks in the HPLC Instrument.

2.40 Impairment of Precision as a Result of Noise.

2.41 Determination of Peak Area and Height at High Noise.

2.42 Peak Height Ratios.

2.43 Incompletely Resolved Peaks.

2.44 Area Rules for Incompletely Resolved Peaks.

2.45 Areas for a 1 : 10 Peak Pair.

2.46 Heights for a 1 : 10 Peak Pair.

2.47 Quantitative Analysis of a Small Peak.

2.48 Incompletely Resolved Peaks with Tailing.

2.49 Integration Threshold and Number of Detected Peaks.

2.50 Detector Time Constant and Peak Shape.

2.51 Quantitative Analysis in the 99 % Range.

2.52 Correlation Coefficient of Calibration Curves.

Part III:Useful Strategies.

3.1 Column Tests.

3.2 Apparatus Tests.

3.3 Wavelength Accuracy of the UV Detector.

3.4 Internal Standards.

3.5 A Linearity Test.

3.6 Rules for Accurate Quantitative Peak Size Determination.

3.7 High-Low Chromatography.

3.8 Control Charts.

3.9 Verification of the Analytical Result by Use of a Second Method.

3.10 Description of Ruggedness.

3.11 Rules for Passing On an HPLC Method.

3.12 Quality Assurance in the Laboratory.

3.13 Standard Operating Procedures.

3.14 Method Validation.

3.15 Some Elements of Validation.

3.16 A Validation Example.

3.17 Measurement Uncertainty.

3.18 Formal Quality Assurance Systems.

Index.

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