- ISBN: 9783527320523 | 3527320520
- Cover: Hardcover
- Copyright: 3/23/2009
Dr. Gjerde received his PhD in analytical chemistry from Iowa State University. After having worked in large and small companies for a number of years, Gjerde founded Sarasep in 1990 for the production and commercialization of polymeric separation technologies. Gjerde has authored and coauthored numerous articles and 4 books and holds nearly fifty patents in separation science.
Preface | p. 13 |
Acknowledgments | p. 15 |
Introduction and Overview | p. 1 |
Introduction | p. 1 |
Historical Development | p. 2 |
Early Ion-Exchange Separations | p. 2 |
Cation Separations | p. 3 |
Separation of Anions | p. 6 |
On-line Detection | p. 8 |
The Birth of Modern Ion Chromatography | p. 8 |
Non-Suppressed-Ion Chromatography | p. 10 |
Principles of Ion Chromatographic Separation and Detection | p. 13 |
Requirements for Separation | p. 13 |
Experimental Setup | p. 13 |
Performing a Separation | p. 14 |
Migration of Sample Ions | p. 15 |
Detection | p. 17 |
Basis for Separation | p. 17 |
Instrumentation | p. 21 |
Components of an Ion Chromatography (IC) Instrument | p. 21 |
General Considerations | p. 23 |
Eluent | p. 24 |
Pump | p. 26 |
Gradient Formation | p. 29 |
Sample Injector | p. 30 |
Columns | p. 31 |
Column Hardware | p. 31 |
Column Protection | p. 32 |
Column Oven | p. 33 |
Two-dimensional IC | p. 33 |
Suppressor | p. 33 |
Detector | p. 34 |
Data Acquisition and Calculation of Results | p. 35 |
Resins and Columns | p. 37 |
Introduction | p. 37 |
Polymeric Resins | p. 38 |
Substrate and Cross Linking | p. 38 |
Microporous Resins | p. 39 |
Macroporous Resins | p. 40 |
Chemical Functionalization | p. 41 |
Resin Capacity | p. 42 |
Resins and Columns for Ion Chromatography | p. 43 |
Monolith Columns | p. 43 |
Anion Exchangers | p. 45 |
Porous Anion Exchangers | p. 45 |
Effect of Functional Group on Selectivity | p. 47 |
Effect of Spacer Arm Length | p. 52 |
Latex Agglomerated Ion Exchangers | p. 54 |
Effect of Latex Functional Group on Selectivity | p. 56 |
Cation Exchangers | p. 57 |
Sulfonated Resins | p. 57 |
Weak-acid Cation Exchangers | p. 61 |
Other Types | p. 63 |
Other Resins | p. 63 |
Chelating Ion-exchange Resins | p. 63 |
Metal Oxides | p. 64 |
Multi-purpose Resins | p. 64 |
Ion-exchange Disks | p. 65 |
Detectors | p. 69 |
Introduction | p. 69 |
Conductivity Detectors | p. 70 |
Conductivity Definitions and Equations | p. 73 |
Principles of Cell Operation | p. 74 |
Conductance Measurement | p. 75 |
Conductivity Hardware and Detector Operation | p. 75 |
Contactless Conductivity Detection | p. 76 |
Ultraviolet-Visible (UV-Vis) Detectors | p. 77 |
UV-Vis measurement | p. 77 |
Direct Spectrophotometric Measurement | p. 78 |
Post-column Derivatization | p. 81 |
UV-Vis Hardware and Detector Operation | p. 82 |
Fluorescence Detector | p. 83 |
Electrochemical Detectors | p. 85 |
Potentiometric Detection | p. 86 |
Conductometric Detectors | p. 86 |
Amperometric/Coulometric Detection | p. 87 |
Pulsed Electrochemical Detection (PED) | p. 89 |
Pulsed Amperometric Detection (PAD) | p. 91 |
Integrated Pulsed Amperometric Detection (IPAD) | p. 93 |
IC-PED | p. 94 |
Post-column Derivatization | p. 95 |
Electrochemical Hardware and Detector Operation | p. 95 |
Refractive Index Detector | p. 97 |
Evaporative Light Scattering Detector (ELSD) | p. 97 |
Nebulizer | p. 98 |
Evaporation Chamber | p. 99 |
Detection Cell | p. 99 |
Other Detectors | p. 100 |
Principles of Ion Chromatographic Separations | p. 105 |
General Considerations | p. 105 |
Chromatographic Terms | p. 105 |
Retention Factor | p. 106 |
Selectivity | p. 109 |
Selectivity Coefficients | p. 110 |
Other Ion-exchange Interactions | p. 112 |
Selectivity of Sulfonated Cation-exchange Resin for Metal Cations | p. 113 |
Factors Affecting Selectivity | p. 120 |
Polymeric Matrix Effect | p. 121 |
Resin Functional Group | p. 122 |
Solvation Effects | p. 123 |
Chromatographic Efficiency | p. 124 |
Anion Chromatography | p. 131 |
Scope and Conditions for Separation | p. 131 |
Columns | p. 132 |
Separation Conditions | p. 135 |
Suppressed Anion Chromatography | p. 138 |
Electrolytic Suppressors | p. 140 |
Solid-Phase Reagents, 1990[7] | p. 141 |
Typical Separations | p. 142 |
Isocratic and Gradient Elution | p. 144 |
Influence of Organic Solvents | p. 146 |
Nonsuppressed Ion Chromatography | p. 147 |
Principles | p. 147 |
Explanation of Chromatographic Peaks | p. 150 |
Eluent | p. 150 |
General Considerations | p. 150 |
Salts of Carboxylic Acids | p. 151 |
Basic Eluents | p. 152 |
Carboxylic Acid Eluents | p. 153 |
System Peaks | p. 154 |
Scope of Anion Separations | p. 155 |
Sensitivity | p. 155 |
Conductance of a Sample Peak | p. 158 |
Coated Columns | p. 160 |
Optical Absorbance Detection | p. 163 |
Introduction | p. 163 |
Direct UV Absorption | p. 163 |
Indirect Absorbance | p. 164 |
Detection | p. 166 |
Pulsed Amperometric Detector (PAD) | p. 168 |
Evaporative Light Scattering Detector (ELSD) | p. 170 |
Inductively Coupled Plasma Methods (ICP) | p. 172 |
Atomic Emission Spectroscopy (AES) | p. 172 |
Inductively Coupled Plasma Mass Spectrometry (ICP-MS) | p. 173 |
Cation Chromatography | p. 175 |
Introduction | p. 175 |
Columns | p. 176 |
Historical Development | p. 178 |
Phosphonate Columns | p. 179 |
Macrocycle Columns | p. 181 |
Surfactant Columns | p. 182 |
Separations | p. 184 |
Suppressed-Conductivity Detection | p. 184 |
Non-Suppressed-Conductivity Detection | p. 187 |
Spectrophotometric Detection | p. 188 |
Effect of Organic Solvents | p. 191 |
Separation of Alkali Metal Ions | p. 193 |
Separation of Metal Ions with a Complexing Eluent | p. 195 |
Principles | p. 195 |
Separations | p. 196 |
Use of Sample Masking Reagents | p. 197 |
Weak-Acid Ion Exchangers | p. 198 |
Chelating Ion-Exchange Resins and Chelation Ion Chromatography | p. 201 |
Fundamentals | p. 201 |
Examples of Metal-Ion Separation | p. 204 |
Ion-Exclusion Chromatography | p. 207 |
Principles | p. 207 |
Equipment | p. 209 |
Eluents | p. 209 |
Detectors | p. 210 |
Separation of Organic Acids | p. 211 |
Effect of Alcohol Modifiers | p. 214 |
Separation of Carboxylic Acids on Unfunctionalized Columns | p. 216 |
Simultaneous Determination of Anions and Cations | p. 217 |
Conclusions | p. 220 |
Determination of Carbon Dioxide and Bicarbonate | p. 222 |
Enhancement Column Reactions | p. 222 |
Separation of Bases | p. 223 |
Determination of Water | p. 226 |
Determination of Very Low Concentrations of Water by HPLC | p. 229 |
Separation of Saccharides and Alcohols | p. 230 |
Introduction | p. 230 |
Separation Mechanism and Control of Selectivity | p. 230 |
Detection | p. 235 |
Contamination | p. 235 |
Ion Pair Chromatography | p. 239 |
Principles | p. 239 |
Typical Separations | p. 242 |
Mechanism | p. 246 |
Zwitterion Stationary Phases | p. 251 |
Introduction | p. 251 |
Simultaneous Separation of Anions and Cations | p. 253 |
Separation of Anions | p. 255 |
Separation of Cations | p. 256 |
Mechanism | p. 259 |
Capillary Electrophoresis | p. 263 |
Introduction | p. 263 |
Steps in Analysis | p. 264 |
Capillary Pretreatment | p. 264 |
Sample Introduction | p. 264 |
Sample Run | p. 265 |
Detection | p. 265 |
Principles | p. 265 |
Terms and Relationships | p. 265 |
Zone Broadening | p. 267 |
Sample Injection | p. 267 |
Electrosmotic Flow (EOF) | p. 268 |
Effect of EOF on Separations | p. 270 |
Control of EOF | p. 271 |
Separation of Ions | p. 274 |
Separation of Anions | p. 274 |
Separation of Isotopes | p. 276 |
Separation of Cations | p. 278 |
Separations at Low pH | p. 279 |
Capillary Electrophoresis at High Salt Concentration | p. 280 |
Capillary Electrophoretic Ion Chromatography | p. 283 |
Micellar Electrokinetic Chromatography (MEKC) | p. 284 |
Partial Complexation | p. 285 |
Effect of Ionic Polymers | p. 287 |
Effect of Alkylammonium Salts | p. 291 |
Separation Mechanism | p. 294 |
Summary | p. 294 |
DNA and RNA Chromatography | p. 299 |
Introduction | p. 299 |
Importance of DNA and RNA Chromatography | p. 299 |
Organization of this Chapter | p. 300 |
DNA and RNA Chemical Structure and Properties | p. 301 |
DNA and RNA Chromatography | p. 303 |
Development of DNA and RNA Chromatography | p. 303 |
Column Properties | p. 305 |
Ion-pairing Reagent and Eluent | p. 306 |
Temperature Modes of DNA and RNA Chromatography | p. 307 |
Nondenaturing Mode | p. 307 |
Fully Denaturing Mode | p. 308 |
Partially Denaturing Mode | p. 309 |
Instrumentation | p. 310 |
Effect of Metal Contamination | p. 310 |
The Column Oven | p. 313 |
UV and Fluorescence Detection | p. 313 |
Fragment Collection | p. 314 |
Applications of DNA Chromatography | p. 314 |
Dhplc | p. 314 |
Nucleic Acid Enzymology | p. 315 |
Telomerase Assays | p. 315 |
Polynucleotide Kinase Assays | p. 316 |
Uracil DNA Glycosylase Assays | p. 317 |
Applications of RNA Chromatography | p. 317 |
Separation of Messenger RNA from Ribosomal RNA | p. 318 |
Analysis of Transfer RNA | p. 319 |
Sample Pretreatment | p. 323 |
Dilute and Shoot or Pre-treat the Sample? | p. 323 |
Particulate and Column-contaminating Matter | p. 324 |
Preconcentration | p. 325 |
Collection of Ions from Air | p. 325 |
Preconcentration of Ions in Water | p. 326 |
Sample Pretreatment | p. 328 |
Anions in Acids | p. 328 |
Neutralization of Strongly Acidic or Basic Samples | p. 328 |
Dialysis Sample Preparation | p. 329 |
Passive Dialysis | p. 330 |
Donnan (Active) Dialysis | p. 330 |
Isolation of Organic Ions | p. 333 |
Method Development and Validation | p. 335 |
Choosing a Method | p. 335 |
Define the Problem Carefully | p. 335 |
Experimental Considerations | p. 336 |
Example of Method Development | p. 338 |
Some Applications of Ion Chromatography | p. 340 |
Statistical Evaluation of Data | p. 341 |
Common Statistical Terms | p. 341 |
Distribution of Means | p. 344 |
Confidence Intervals | p. 345 |
Validation of Analytical Procedures | p. 347 |
Analytical Control | p. 349 |
Chemical Speciation | p. 353 |
Introduction | p. 353 |
Detection | p. 355 |
Chromatography | p. 356 |
Valveless Injection IC | p. 357 |
Speciation of some Elements | p. 359 |
Chromium | p. 359 |
Iron | p. 360 |
Arsenic | p. 361 |
Tellurium | p. 362 |
Selenium | p. 363 |
Vanadium | p. 364 |
Tin | p. 364 |
Mercury | p. 365 |
Other Metals | p. 365 |
Index | p. 369 |
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