Chromatographic Integration Methods

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ISBN: 9780854045105 | 0854045104
Cover: Hardcover
Copyright: 8/1/1998

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The second edition of the popular Chromatographic Integration Methods has been completely revised and updated. Written by an expert with many years' experience with two of the world's largest manufacturers of computing integrators, it has been expanded to include a new section on validation of integrators in response to regulatory requirements for quality and validation. A new literature survey, additional diagrams and Author Index have also been added. Well illustrated and easily read, this is an excellent source book for those who wish to increase their understanding of integrators. Chromatographic Integration Methods describes and discusses both manual and electronic techniques used, with the aim of aiding analysts to obtain more data from their chromatograms, and assist them with understanding how integrators work so that results are never accepted unquestioningly. As with the first edition, this book will be welcomed by all those in the chromatography field, particularly those at the bench.

Measurements and Models

(34)

The Basic Measurements

(1)

Measurements and Their Use

(1)

Quantitation

(3)

Peak Area and Peak Height

(2)

Peak `Volume'

(1)

Retention Time and Solute Identity

(1)

Column Hold-Up Time

(1)

Diagnostics and System Suitability Tests

(6)

Baseline Noise

(1)

Baseline Signal Level

(1)

Peak Boundaries

(1)

Peak Width and Column Efficiency

(1)

Peak Asymmetry

(2)

Peak Resolution

(1)

Retention Time Stability

(1)

Results Assessment

(1)

Correct Peak Measurements

(1)

Total Peak Area

(1)

Correct Number of Peaks

(1)

Coefficient of Variation and Relative Standard Deviation

(1)

Comparison Against Standards

(1)

Trend Analysis

(1)

Performance Measurement

(1)

Chromatograph Utilization

(1)

Analyst Workload

(1)

Cost per Analysis

(1)

Chromatographic Peak Models

(11)

The Gaussian Function

(1)

The Function

(1)

Peak Height

(1)

Ratio of Area/Height

(1)

Calculation of Peak Width at Various Heights

(1)

Gaussian Peak Shape Tests

(1)

The Points of Inflection

(1)

Fractional Peak Area Bounded by Various Widths

(1)

Loss of Area from the Base of a Gaussian Peak

(1)

Gaussian Peak Maximum as an Approximate Parabola

(2)

The Exponentially Modified Gaussian Function

(1)

The Function

(2)

Practical Application of the EMG Function

(1)

EMG Peak Shape Tests

(1)

Statistical Moments of a Chromatographic Peak

(5)

Zeroeth Moment, m0

(1)

First Moment, m1

(1)

Second Moment, m2

(1)

Third Moment, m3

(1)

Fourth Moment, m4

(1)

Higher Odd Moments

(1)

Higher Even Moments

(1)

Measurements of Peak Moments

(1)

Practical Disadvantages and Uses

(1)

Manual Peak Area Measurement

(5)

Height X Width at Half Height

(1)

The Condal-Bosch Area

(1)

Peak Area by Triangulation

(1)

Manual Measurement of Asymmetric (EMG) Peaks

(2)

References

(2)

Errors in Peak Area Measurement

(54)

Accuracy and Precision

(4)

Accuracy

(1)

Precision

(1)

Inaccuracy and Uncertaintly

(1)

Repeatability

(1)

Reproducibility

(1)

Random Errors

(1)

Systematic Errors

(1)

Spurious Errors

(1)

Causes of Imprecision

(1)

Causes of Inaccuracy

(1)

Precision of Integrator Measurements

(2)

Accurate Representation of the Solute Profile

(4)

Additivity of Signals

(1)

Negative Detector Signals

(1)

Electronic Peak Distortion

(2)

Peak Area and Solute Quantity

(7)

Mass and Flow Sensitive Detectors

(1)

Flow Sensitive Detectors

(1)

Mass Sensitive Detectors

(2)

Detector Overload

(1)

Linearity

(1)

Detector Non-linearity

(1)

Column Non-linearity

(1)

Electronic Noise and Drift

(1)

Sources of Peak Measurement Error

(36)

Hardware Errors

(1)

Noise

(1)

Noise and Frequency

(1)

Short-term Noise

(1)

Long-term Noise

(1)

Drift

(2)

Errors Created by Noise

(1)

Signal-to-noise Ratio: The Smallest Measurable Peak

(1)

Limits of Detection and Quantitation

(1)

A `Good Baseline'

(1)

Errors Created by Baseline Drift

(1)

Drifting Baseline and Peak Measurement

(2)

Baseline Drift and Retention Time

(1)

Reduced Detector Operating Range

(1)

Some Preliminary Conclusions

(1)

Errors of Incomplete Peak Resolution

(2)

Height of a Fused Peak

(1)

Perpendicular Separation

(2)

Effect of Overlap on Area Measurement Accuracy

(3)

Error Correction Strategies

(1)

Error Propagation through Overlapping Groups

(2)

Peak Overlap and Calibration

(1)

Tangent Skim Errors

(1)

Errors of Perpendicular/Tangent Transition

(1)

Overlapping Peaks on Sloping Baselines

(2)

Multiple Fused Peaks

(2)

Mathematical Deconvolution of Overlapping Peaks

(1)

The Isomer Test

(1)

Errors from Peak Asymmetry

(1)

Asymmetry and Peak Tailing

(2)

Asymmetry and Base Broadening

(1)

Asymmetry and Manual Peak Measurement

(1)

Unequal Asymmetry

(1)

The Achievement of Accuracy in Chromatographic Analyses

(1)

Peak Area vs. Peak Height

(2)

User Surveys

(1)

References

(3)

Manual Measurement of Peaks

(18)

Representation of the Detector Signal by Chart Recorder

(3)

Slow Response Time

(1)

Non-linear Signal Response

(1)

Pen Head Damping

(1)

Amplifier Noise

(1)

Manual Measurement of Noise

(1)

Dead Band

(1)

Chart Motor Control

(1)

Attenuator Accuracy

(1)

Measurement Strategies

(2)

Counting Squares

(1)

Cutting and Weighing

(1)

Planimeters

(1)

Measurements based on a Peak Model

(7)

Pencil and Rule Methods

(1)

Measurement of Peak Height

(1)

Height vs. Area Measurements

(1)

Triangulation

(1)

Peak Height X Width at Half Height

(1)

Condal-Bosch Variation

(1)

The Foley Variations

(2)

Measurement of Overlapping Asymmetric Peaks

101

(1)

Peak Shape Tests

101

(1)

Errors of Manual Measurement

101

(4)

Optimum Peak Shape

103

(2)

Advantages and Disadvantages of Manual Peak Measurement

105

(1)

References

105

(2)

Digital Integrators

107

(33)

A Brief History of Integrators

107

(5)

Strip Chart Recorder Techniques

107

(1)

Electromechanical Counters

107

(3)

Electronic Integrators

110

(1)

TTL Instruments-The First Electronic Integrators

110

(1)

Microprocessor-based Integrators

111

(1)

Integrators with Printer Plotters

111

(1)

The Impact of the Microcomputer

112

(1)

Current Integrator Status

112

(17)

Standard Integrator Specification

113

(1)

Integrator Files

114

(1)

Analysis Parameters for Peak Measurement

114

(1)

Peak Width

115

(1)

Slope Sensitivity or Detection Threshold

115

(2)

Baseline Drift Tolerance

117

(1)

Time to Double

117

(1)

Minimum Area or Height Threshold

118

(1)

Analysis Duration

118

(1)

Integrate Inhibit

118

(1)

Forcing Tangent or Perpendicular Separation

118

(2)

Forcing Baseline Detection

120

(1)

Horizontal Baseline Projection

120

(2)

Inverting Negative Peaks

122

(1)

Instrument Control and Communications

123

(1)

Sample Management, Calculations and Calibrations

123

(1)

Peak and Solute Identity

123

(1)

Relative Retention Times

124

(1)

Standard Calculations

124

(1)

Area% or Normalization

124

(1)

Internal Standard

125

(1)

External Standard

125

(1)

Sample Scheduling

126

(1)

Calibration

126

(1)

Report Preparation and Output

127

(1)

Trends

128

(1)

Report Distribution

128

(1)

Validation of Integrators

129

(6)

The Integrator as a Diagnostic Tool

129

(1)

Specification, Installation, Operational, Performance Qualification

130

(1)

Integrator Specification and Selection (SQ)

130

(1)

Installation Checks (IQ)

131

(1)

Operational Qualification (OQ)

132

(1)

Validation and Calibration: The Difference

132

(1)

Records

132

(1)

Performance Qualification (PQ): Regular Testing of the Integrator

133

(1)

Logging Results

134

(1)

Validation of Software

134

(1)

Standard Chromatograms

135

(3)

Creation of Standard Chromatograms

136

(1)

Computer-based Standard Chromatograms

136

(1)

Specification of Standard Chromatograms

137

(1)

Creation of Synthetic Chromatograms

137

(1)

Baselines

137

(1)

Baseline Noise

137

(1)

Drift

138

(1)

Traceability of Synthetic Chromatograms

138

(1)

References

138

(2)

Digital Measurement of Peak Areas

140

(53)

Signal Sampling

140

(10)

Analogue to Digital Conversion

140

(1)

Voltage to Frequency Conversion

140

(1)

Dual Slope, Integrating A/D Conversion

141

(2)

Resolution of A/D Converters

143

(1)

Auto-ranging of A/D Converters

143

(1)

Data Sampling Frequency

144

(1)

Sampling Frequency and Integrator Manufacture

144

(1)

Sampling Frequency and Data Processing Algorithms

144

(1)

Data Bunching

144

(1)

Baseline Bunching

145

(1)

Estimating the A/D Sampling Frequency and Bunch Size

146

(2)

Data Bunching and the Peak Width Parameter

148

(1)

Peak Width Parameter and Analysis Reprocessing

148

(1)

Peak Sampling Synchronization

149

(1)

Rounding or Truncation Errors

149

(1)

Aperture Time Jitter

149

(1)

Filtering and Smoothing the Chromatographic Signal

150

(8)

Filtering

150

(1)

Smoothing

150

(1)

Electronic Filters

150

(1)

Sampling Frequency and Mains Coupling

150

(1)

Smoothing Techniques

151

(1)

Digitizing and Integrating

151

(1)

Bunching

151

(2)

Moving Windows and Polynomail Curve Fitting

153

(1)

Optimum Filtering

154

(1)

Signal Subtraction

155

(2)

Chromatogram Plotting

157

(1)

Matched Filtering

157

(1)

Location and Measurement of Peaks

158

(17)

Finding the Peaks

159

(1)

Retention Time

160

(1)

Peak Shape Test

160

(1)

Properties of the Smoothed Data

160

(1)

Data Integrals

161

(1)

Baseline Fluctuations and Slope Sensitivity

162

(1)

Programming Slope Sensitivity

162

(1)

Slope Sensitivity and Representative Baseline

162

(1)

Updating Peak Width and Slope Sensitivity during Analyses

163

(1)

Location of the Limits of Integration

163

(2)

Small Peak Filtering

165

(1)

Location of Peak End

165

(1)

Measurement of Peak Area

166

(2)

Baseline Convention

168

(1)

Measurement of Peak Height

168

(1)

Measurement of Retention Time

168

(1)

Measurement of Two Unresolved Peaks

169

(1)

Measurement of Individual Peak Areas

170

(1)

Peak Measurement Diagnostics

170

(1)

Measurement of Fused Groups

170

(1)

Shoulders

171

(1)

Measurement of Tangent Peaks

172

(1)

Tangent Skimmed Groups

173

(1)

Small Peaks between Larger Ones

174

(1)

Tangents on Tangents

175

(1)

Baselines, A More Detailed Discussion

175

(15)

Baseline Drift Limit

175

(2)

False Starts

177

(1)

Formulating a Baseline Definition

177

(1)

Mis-timing `Start' and `End'

178

(1)

End of `Integrate Inhibit'

178

(1)

Forcing Baseline

179

(1)

Incorrect Programming of Baseline Drift Tolerance

180

(2)

Fused Tangent Measurement

182

(1)

Single Peaks on a Rising Baseline

183

(1)

Valleys Between Fully-resolved Peaks

184

(1)

Negative Dips and Constructed Baselines

184

(3)

Assigning Baseline Beneath the Whole Chromatogram

187

(3)

Valley-Valley Skim

190

(1)

Conclusions

190

(1)

References

191

(2)

Author Index

193

(3)

Subject Index

196

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Chromatographic Integration Methods

Summary

Table of Contents

Supplemental Materials

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Chromatographic Integration Methods

Summary

Table of Contents

Supplemental Materials

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