Pitfalls and Errors of HPLC in Pictures (Desk Library of Chemistry Series) / Edition 1

Pitfalls and Errors of HPLC in Pictures (Desk Library of Chemistry Series) / Edition 1

by Veronika R. Meyer
     
 

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ISBN-10: 3527297170

ISBN-13: 9783527297177

Pub. Date: 10/28/1999

Publisher: Wiley

Errors are a common companion of all human acitvity, including work in the laboratory. Yet it is a great pity if erroneous results are produced with great effort and by using expensive instruments and demanding procedures. Therefore a book about sources of errors in high performance liquid chromatography, today's most widely used analytical method, is highly

Overview

Errors are a common companion of all human acitvity, including work in the laboratory. Yet it is a great pity if erroneous results are produced with great effort and by using expensive instruments and demanding procedures. Therefore a book about sources of errors in high performance liquid chromatography, today's most widely used analytical method, is highly recommended. Maybe the topic is not welcomed enthusiastically but, nevertheless, it is nessecary.
In conception, at least, possibe problems can be devided into two categories. "Errors" are troublesome opponents of accurate and precise results which, however, can be understood. In contrast, "pitfalls" are totally unexpected intruders and the secret behind them is difficult to discover. The worst are those which are not detected but which affect the result anyway.
The book does not, nevertheless, distinguish between the two types. The reader decide how they classify them. The single topics were presented in a clearly arranged style: a brief text with a corresponding figure which should encourage reading and thinking.
Chemists and laboratory assistants get numerous hints how correct and reliable results could be transposed in daily laboratory work.

Product Details

ISBN-13:
9783527297177
Publisher:
Wiley
Publication date:
10/28/1999
Series:
Desk Library of Chemistry Series
Pages:
168
Product dimensions:
5.94(w) x 9.25(h) x 0.52(d)

Table of Contents

Preface
Introduction
PART I: FUNDAMENTALS
Chromatography
Chromatographic figures of merit
The resolution of two peaks
Reduced parameters
The van Deemter curve
Peak capacity and Number of Possible Peaks
Statistical resolution probability: Simulation
Statistical resolution probability: Example
Precision and accuracy of an analytical result
The propagation of random errors
Reproducibility in trace analysis
Ruggedness
Calibration curves
The HPLC instrument
The detector response curve
Noise
PART II: PITFALLS AND SOURCES OF ERROR
Mixing of the mobile phase
Mobile phase pH
Adjustment of mobile phase pH
Inadequate purity of reagents or solvents
System peaks and quantitative analysis
Sample preparation with solid phase extraction
Poor choice of sample solvent and calibration curve
Impurities in the sample
Formation of a by-product in the sample solution
Formation of an associate in the sample solution
Precision and assuracy with loop injection
Injection technique
Injection of air
Sample adsorption in the loop
Extra-column volumes
Dwell volume
Elution at t0
Classification to C18 reversed phases
Different batches of stationary phase
Chemical reaction within the column
Double peaks from stable conformers
Influence of temperature on the separation
Influence of the volume flow rate on the separation
Influence of run time and volume flow rate on gradient separations
UV detection wavelength
Detector overload
Influence of the capacity factor on peak height
Influence of the volume flow rate on peak area
Leaks in the HPLS instrument
Impairment of precision as a result of noise
Determination of peak area and height at high noise
Peak height ratios
Incompletely resolved peaks
Area rules for incompletely resolved peaks
Areas for a 1 : 10 peak pair
Heights for a 1 : 10 peak pair
Quantitative analysis of a small peak
Incompletely resolved peaks with tailing
Quantitative analysis in the 99% range
Correlation coefficient of calibration curves
PART III: USEFUL STRATEGIES
Column tests
Apparatus tests
Wavelength accuracy of the UV detector
Internal standards
Ruels for accurate quantitative peak size determination
High-low chromatography
Control charts
Verification of the analysis result by use of a second method
Description of ruggedness
Rules for passing on an HPLC method
Quality assurance in the laboratory
Standard operating procedures
Method validation
Formal quality assurance systems
Index

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