ISBN: 3-540-64007-X
TITLE: Principles of Analytical Chemistry
AUTHOR: Valcarcel, Miguel
TOC:

1 Introduction to Analytical Chemistry 1 
1.1 Analytical Chemistry Today 1 
1.2 Analytical Chemical Information 6 
1.3 Analytical Chemical References 10 
1.4 Essential Features of Analytical Chemistry 11 
1.4.1 Basic Elements 12 
1.4.2 Fundamentals 13 
1.4.3 Key Words 14 
1.4.4 Developments 15 
1.4.5 Placement 17 
1.4.6 Boundaries 18 
1.5 Evolution of Analytical Chemistry 19 
1.6 Conceptual and Technical Hierarchies 22 
1.7 Classifications 28 
Questions 34 
Seminars 36 
Suggested Readings 37 
2 Analytical Properties 39 
2.1 Introduction 40 
2.2 The Chemical Metrological Hierarchy: Uncertainty and Trueness 41 
2.3 Errors in Analytical Chemistry 45 
2.4 Capital Analytical Properties 52 
2.4.1 Accuracy 53 
2.4.2 Representativeness 54 
2.5 Basic Analytical Properties 56 
2.5.1 Precision 57 
2.5.2 Sensitivity 65 
2.5.3 Selectivity 69 
2.6 Accessory Analytical Properties 72 
2.6.1 Expeditiousness 73 
2.6.2 Cost-effectiveness 73 
2.6.3 Personnel-related Factors 75 
2.7 Relationships among Analytical Properties 75 
2.7.1 Hierarchical Relationships 76 
2.7.2 Foundation Relationships 77 
2.7.3 Contradictory Relationships 77 
2.7.4 Complementary Relationships 81 
2.8 Other Analytical Properties 83 
Questions 87 
Seminars: Numerical Problems 89 
Suggested Readings 100 
3 Traceability: Reference Materials 101 
3.1 Introduction 102 
3.2 The Integral Concept of Traceability 102 
3.3 Physical and Chemical Traceability 105 
3.4 Types of Standards and their Traceability 107 
3.5 Analytical Chemical Standards 112 
3.5.1 Types 113 
3.5.2 General Properties 116 
3.5.3 Preparation and Storage 119 
3.5.4 Uses 122 
3.5.4.1 Calibration of Equipment and Methods 123 
3.5.4.2 Evaluation of Analytical Processes 128 
3.6 Specific Meanings of Traceability 130 
3.6.1 Traceability of an Analytical Result 130 
3.6.2 Traceability of a Sample (Aliquot) 132 
3.6.3 Traceability of an Instrument 134 
3.6.4 Traceability of a Sample Standard 134 
3.6.5 Traceability of a Method 135 
3.6.6 Relationships among Traceability Meanings 135 
Questions 137 
Seminars 139 
Suggested Readings 141 
4 The Measurement Process in Chemistry 143 
4.1 Definition of Chemical Measurement Process 144 
4.2 General Steps of a Chemical Measurement Process 147 
4.3 Preliminary Operations 149 
4.3.1 General Features 150 
4.3.2 Sub-steps 154 
4.3.3 Sampling 155 
4.3.4 Sample Treatment 161 
4.4 Measurement and Transducing of the Analytical Signal 168 
4.5 Signal Acquisition and Data Processing 171 
4.6 Validation of a Chemical Measurement Process 173 
4.7 Salient Current Trends 174 
Annex I 177 
Annex II 182 
Annex III 186 
Annex IV 189 
Annex V 190 
Annex VI 192 
Questions 194 
Seminars 196 
Suggested Readings 199 
5 Qualitative Aspects of Analytical Chemistry 201 
5.1 Introduction 202 
5.2 The Binary Response 203 
5.2.1 Types of Binary Response 204 
5.2.2 Quantitative Connotations 205 
5.2.3 Analytical Features 208 
5.2.4 Errors: False Positives and False Negatives 210 
5.3 Types of Qualitative Identification 212 
5.4 Standards and Calibration in Qualitative Analysis 214 
5.5 Classical Qualitative Analysis 215 
5.5.1 General Notions 215 
5.5.2 Types of Reagents 217 
5.5.3 Analytical Schemes 221 
5.5.3.1 Schemes without Group Separation 222 
5.5.3.2 Schemes with Group Separation 224 
5.6 Instrumental Qualitative Analysis 229 
5.6.1 General Notions 229 
5.6.2 Static Systems 232 
5.6.3 Dynamic Systems 235 
Questions 240 
Seminars 242 
Suggested Readings 244 
6 Quantitative Aspects of Analytical Chemistry 247 
6.1 Fundamentals 248 
6.1.1 Introduction 248 
6.1.2 Analytical Properties 249 
6.1.3 Equipment and Method Calibration 249 
6.1.4 Classical and Instrumental Quantitative Analysis 250 
6.1.5 Quantitation Methodologies 252 
6.1.6 Expressing Quantitative Results 253 
6.2 Calculable Quantitation Methods 256 
6.2.1 Absolute Methods Involving no Analytical Standard 257 
6.2.1.1 Gravimetry 259 
6.2.1.2 Coulometry 262 
6.2.2 Absolute Methods Involving Analytical Standards 263 
6.2.2.1 Isotope Dilution Mass Spectrometry 263 
6.2.2.2 Titrimetry 264 
6.3 Relative Quantitation Methods 271 
6.3.1 Interpolation and Extrapolation Methods 271 
6.3.2 Comparative Methods 275 
Questions 276 
Seminars 278 
Suggested Readings 281 
7 The Analytical Problem 283 
7.1 Introduction 283 
7.2 Meanings of "Problem" in Analytical Chemistry 286 
7.3 Integral Definition of the Analytical Problem 286 
7.4 Elements of the Analytical Problem 289 
7.5 Steps of the Analytical Problem-solving Process 290 
7.5.1 Identifying and Confirming the Information Required 291 
7.5.2 Pinpointing the Analytical Information Required 292 
7.5.3 Planning the Analytical Approach 294 
7.5.4 Monitoring the Results 296 
7.5.5 Implementing Corrective Actions 297 
7.6 Consistency Between Required Information and Supplied 
Information 297 
7.7 The Analytical Problem in the Context of Quality 299 
Questions 301 
Seminars 304 
Suggested Readings 305 
8 Analytical Chemistry and Quality 307 
8.1 Introduction 308 
8.2 A Generic Approach to Quality 310 
8.2.1 Integral Definition of Quality 310 
8.2.2 Types of Quality 313 
8.2.3 Quality Compromises 314 
8.2.4 Structure of Quality 315 
8.2.5 Benefits of Quality 316 
8.3 General Aspects of Quality in Analytical Chemistry 317 
8.3.1 Types of Quality in Analytical Chemistry 317 
8.3.2 Quality and Analytical Properties 318 
8.3.3 Quality and the Analytical Problem 319 
8.4 Quality Systems in the Analytical Laboratory 319 
8.4.1 Elements of Quality Assurance 319 
8.4.2 ISO Guide 25 (EN-45000) 321 
8.4.3 Good Laboratory Practices 323 
8.4.4 Specific Quality Systems Used in Analytical Chemistry 324 
8.5 Analytical Quality Control 326 
8.6 Assessment of Analytical Quality 327 
8.6.1 Types of Assessment Systems 327 
8.6.2 Laboratory Accreditation 330 
8.6.3 Proficiency Testing 331 
8.7 Supports of Analytical Quality Assurance 334 
8.8 Costs and Benefits of Analytical Quality Systems 336 
Questions 339 
Seminars 341 
Suggested Readings 341 
Glossary of Terms 345 
Symbols and Abbreviations used in the text 367 
END
