Frans_M_Everaerts_Isotachophoresis_378342.pdf

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UV ABSORPTION METER 153 -_-.- +- R - V 0.1 Zero 10MR l00mV Int 1 (6.14) The potentiometers ‘Zero’ and ‘En’ must be arranged in a position such that during the analysis the output voltage on ‘Lin’ always remains between 0 and 100 mV. An example of the linearity of the circuit shown in Fig.6.18 is given in Fig.6.20, in comparison with that of the older circuits. Most of the isotachopherograms considered in this chapter were obtained with non-linear circuitry, but the data collected for the various operational systems that are given in Chapters 11-17 were obtained with linear circuitry. At a resistance of 1 MR, the accuracy of the resistance determination with linear circuitry is better than 2 kf2, whde at 10 MR the accuracy is better than 30 kR. If the ambient temperature increases by 10°C, the difference in resistance determination at a level of 1 Mi2 is less than 1 kR and at 10 Mi2 it is less than 20 kR. The stepwise trace obtained during an isotachophoretic analysis when the zones pass the conductimeter can easily be interpreted for qualitative and quantitative information, because the steps are sufficiently sharp. This is in contrast with thermometric recording. Two main reasons can be given why a differentiator was constructed. (1) If small zones are present, stacked between the others, these zones can be detected much easier and better with an electronic differentiator. (2) If electronic devices are available and applied for measuring the time interval between two successive peaks, a pulse is needed for the printer. A possible circuit for such a differentiator is given in Fig.6.21. The circuit with IC6 is actually the differentiator. Its amplification can be chosen by the potentiometer ‘Diff. The time constant is 24 msec, which is small enough to differentiate the signal on the output ‘En’. The circuit IC7 and lCs is a double-phase rectifier. A potential recorder with a sensitivity of 100 mV can be applied in combination with ths differentiator. IC9 forms, together with the two resistors on the non-inverting input, a Schmitt trigger with a very small hysteresis. The 10-pF capacitor ensures that the input signal is equal to the first differential of the output signal of the rectifier. If this value is zero, the Schmitt trigger is triggered. This procedure is shown schematically in Fig.6.22. The printed values of the time intervals between the fast moving (about 1 m/h) zone boundaries increase the accuracy of time recording and hence the quantitative data handling and, moreover, simplifies the latter. The accuracy in time recording is better than 10 msec, which represents an accuracy of 5 - g-equiv./l, assuming an electric driving current of 70 /.LA and a concentration of the leading electrolyte of lo-* g-equiv./l. 6.5. UV ABSORPTION METER 6.5.1. Introduction Because in the steady state of an isotachophoretic separation all components move in individual zones with identical speeds and only the counter ion is mixed with these components, specific detectors such as the W absorption meter can offer much additional
Fig.6.21. Differentiator for the a.c. conductivity detector and the circuit that produces signals suitable for the printing of the various zone transitions needed for the quantitative measurements. This circuit can be used in combination with the circuit given in Fig.6.18. 154 DETECTION SYSTEMS
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Journal of Chromatogaphy Library -
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Journal of Chromatography Library -
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Dedicated to Pr0f.Dr.h. A.I.M. Keul
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Contents Preface ..................
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CONTENTS IX 6.4.2. The d.c. method
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CONTENTS XI 12.2.2. Applications ..
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It is very well known that charged
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Chapter 1 Historical review SUMMARY
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HISTORICAL REVIEW 3 Independently i
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THEORY
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Chapter 2 Principles of electrophor
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MOVINGBOUNDARY ELECTROPHORESIS a S
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MOVINGBOUNDARY ELECTROPHORESIS 0 iu
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ISOTACHOPHORESIS 13 2.4. PRINCIPLE
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ISOTACHOPHORESIS 15 As the anionic
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ISOTACHOPHORESIS velocities, so tha
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ISOTACHOPHORESIS 19 d.t ’.t I Fig
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ISOTACHOPHORESIS 21 t Fig.2.8. Isot
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ISOELECTRIC FOCUSING 23 The four is
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DISCUSSION 25 Fig.2.11. Survey of t
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Chapter 3 Concept of mobility SUMMA
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IONIC MOBILITY AND IONIC EQUIVALENT
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EFFECTIVE IONIC MOBILITY 31 obtain
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EFFECTIVE IONIC MOBILITY 33 compari
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EFFECTIVE IONIC MOBILITY Fig.3.4. R
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DETERMINATION OF IONIC MOBILITIES 3
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DETERMINATION OF IONIC MOBILITIES 3
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Chapter 4 Mathematical model for is
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GENERAL EQUATIONS 43 anionic specie
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GENERAL EQUATIONS 4.2.1. Equilibriu
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GENERAL EQUATIONS 41 i Similar equa
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GENERAL EQUATIONS 49 Uthzone (U-llt
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GENERAL EQUATIONS 4.2.4. Modified O
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GENERAL EQUATIONS TABLE 4.2 REDUCED
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MATHEMATICAL MODEL FOR THE STEADY S
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VALIDITY OF THE ISOTACHOPHORETIC MO
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CHECK OF THE ISOTACHOPHORETIC MODEL
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CHECK OF THE ISOTACHOPHORETIC MODEL
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REFERENCES 81 Fig.4.17. Relationshi
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Chapter 5 Choice of electrolyte sys
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CHOICE OF THE SOLVENT 85 In general
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CHOICE OF THE SOLVENT TABLE 5.2 THE
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CHOICE OF THE SOLVENT pH and pKvalu
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CHOICE OF THE SOLVENT 91 TABLE 5.4
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CHOICE OF THE pH OF THE LEADING ELE
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CHOICE OF THE pH OF THE LEADING ELE
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CHOICE OF THE TERMINATING AND LEADI
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ADDITIONS TO THE ELECTROLYTE SOLUTI
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EXAMPLES Choice of solvent. Can wat
Page 118 and 119: EXAMPLES 103 solvent, hoping that a
Page 120 and 121: EXAMPLES TABLE 5.11 STEP HEIGHTS OF
Page 122 and 123: EXAMPLES TABLE 5.12 STEP HEIGHTS OF
Page 124 and 125: Fig.5.9. Isotachopherograms of the
Page 126 and 127: EXAMPLES II 4 3 Fig.5.11. Isotachop
Page 128 and 129: REFERENCES 113 Example I. As exampl
Page 130 and 131: INSTRUMENTATION
Page 132 and 133: Chapter 6 Detection systems SUMMARY
Page 134 and 135: THERMOMETRIC RECORDING 6.1.3. Combi
Page 136 and 137: THERMOMETRIC RECORDING Potential gr
Page 138 and 139: THERMOMETRIC RECORDING /2 Fig.6.1.
Page 140 and 141: THERMOMETRIC RECORDING T t l Fig.6.
Page 142 and 143: THERMOMETRIC RECORDING 7 127 It-- I
Page 144 and 145: THERMOMETRIC RECORDING a concentrat
Page 146 and 147: HIGH-FREQUENCY CONDUCTIVITY DETECTI
Page 148 and 149: CONDUCTIVITY DETECTION 133 Fig.6.9.
Page 150 and 151: CONDUCTIVITY DETECTION 135 The d.c.
Page 152 and 153: CONDUCTIVITY DETECTION 137 Hi V 1kR
Page 154 and 155: CONDUCTIVITY DETECTION Fig.6.12. Co
Page 156 and 157: CONDUCTIVITY DETECTION Fig.6.14. Th
Page 158 and 159: CONDUCTIVITY DETECTION 143 6.4.4. T
Page 160 and 161: CONDUCTIVITY DETECTION 145 contact
Page 162 and 163: CONDUCTIVITY DETECTION 147 We can n
Page 164 and 165: CONDUCTIVITY DETECTION 149 N.Y., U.
Page 166 and 167: CONDUCTIVITY DETECTION 151 achieved
Page 170 and 171: UV ABSORPTION METER Fig.6.22. Contr
Page 172 and 173: W ABSORPTION METER r +15V -15V Mod
Page 174 and 175: W ABSORPTION METER 159 TABLE 6.4 PR
Page 176 and 177: W ABSORPTION METER 230 240 2% m zm
Page 178 and 179: to Mod (Fig 6.24) oscillator I sync
Page 180 and 181: UV ABSORPTION METER 165 dicular to
Page 182 and 183: Fig.6.31. Isotachopherograms for th
Page 184 and 185: UV ABSORPTION METER 169 50 Fig.6.33
Page 186 and 187: ADDITIVES TO THE ELECTROLYTES 171 6
Page 188 and 189: ADDITIVES TO THE ELECTROLYTES 173 e
Page 190 and 191: ADDITIVES TO THE ELECTROLYTES 175 a
Page 192 and 193: ADDITIVES TO THE ELECTROLYTES 177 o
Page 194 and 195: ADDITIVES TO THE ELECTROLYTES 179 d
Page 196 and 197: ADDITIVES TO THE ELECTROLYTES 181 T
Page 198 and 199: ADDITIVES TO THE ELECTROLYTES Fig.6
Page 200 and 201: ADDITIVES TO THE ELECTROLYTES 185 F
Page 202 and 203: ADDITIVES TO THE ELECTROLYTES 1 2 3
Page 204 and 205: ADDITIVES TO THE ELECTROLYTES 189 n
Page 206 and 207: COATING OF THE MICRO-SENSING ELECTR
Page 208 and 209: DETECTION LIMITS 193 electric drivi
Page 210 and 211: DETECTION LIMITS 195 Fig.6.48. Infl
Page 212 and 213: DETECTION LIMITS 197 TABLE 6.6 SURV
Page 214 and 215: CONCLUSION 199 average length of a
Page 216 and 217: REFERENCES 201 seen. Again it is cl
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Chapter 7 Instrumentation SUMMARY T
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INJECTION SYSTEMS I! I n Fig.7.1. P
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INJECTION SYSTEMS Fig.7.3. Exploded
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INJECTION SYSTEMS Fig.7.5. Injectio
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COUNTER ELECTRODE COMPARTMENTS 21 1
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COUNTER ELECTRODE COMPARTMENTS Even
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COUNTER ELECTRODE COMPARTMENTS 21 5
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EQUIPMENT the large bore, a more di
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EQUIPMENT 219 belonging to three cl
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EQUIPMENT 221 signal of the thermoc
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EQUIF'MENT 223 No effect on the res
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EQUIPMENT 225 Fig.7.14. Electrophor
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EQUIPMENT Fig.7.16. Photograph of t
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EQUIPMENT 229 mounted equiplanar, w
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COUNTER FLOW OF ELECTROLYTE 231 ins
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COUNTER FLOW OF ELECTROLYTE p High
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COUNTER FLOW OF ELECTROLYTE Fig.7.2
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COUNTER FLOW OF ELECTROLYTE 231 aro
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COUNTER FLOW OF ELECTROLYTE p high
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COUNTER FLOW OF ELECTROLYTE 24 1 7.
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COUNTER FLOW OF ELECTROLYTE I I 31
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COUNTER FLOW OF ELECTROLYTE max. 15
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APPLICATIONS
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Chapter 8 Introduction SUMMARY In t
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INTRODUCTION 25 1 the various ionic
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Chapter 9 Practical aspects SUMMARY
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DISTURBANCES CAUSED BY H+ AND OH 25
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DISTURBANCES CAUSED BY H+ AND OH- 2
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DISTURBANCES DUE TO CO, 263 Electro
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ENFORCED ISOTACHOPHORESIS 265 t T T
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WATER AS TERMINATOR 267 function of
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PURIFICATION OF THE TERMINATOR 7 4
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REFERENCES 271 AS an example, the c
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Chapter 10 Quantitative aspects SUM
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THERMOMETRIC MEASUREMENTS 215 vj c
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THERMOMETRIC MEASUREMENTS TABLE 10.
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CONDUCTIMETRIC MEASUREMENTS factor
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CONCLUSION 28 1 Tables 10.3-10.5 wa
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Chapter 11 Separation of cationic s
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SEPARATION USING A THERMOCOUPLE AS
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I SEPARATION USING A THERMOCOUPLE A
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SEPARATION USING CONDUCTIVITY AND U
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Chapter I2 Separation of anionic sp
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SEPARATION USING A THERMOMETRIC DET
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SEPARATION USING CONDUCTIVITY AND W
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Chapter 13 Amino acids, peptides an
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AMINO ACIDS TABLE 13.1 OPERATIONAL
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AMINO ACIDS 8- ?- 6- 5- 4- 3- 2- f-
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AMINO ACIDS 317 TABLE 13.5 STEP HEI
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AMINO ACIDS Fig.13.3. Schematic dia
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AMINO ACIDS TABLE 13.6 DETERMINATIO
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SEPARATION OF PROTEINS IN AMPHOLYTE
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SEPARATION OF SMALL PEPTIDES reprod
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Chapter I4 Separation of nucleotide
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Chapter 15 Enzymatic reactions SUMM
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ENZYMATIC CONVERSION OF GLUCOSE (FR
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ENZYMATIC CONVERSION OF PYRUVATE 35
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Chapter 16 Separations in non-aqueo
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SEPARATION OF ANIONIC SPECIES IN ME
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SEPARATION OF CATIONIC SPECIES IN M
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EXPERIMENTS IN AQUEOUS METHANOLIC S
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Chapter I7 Counter flow of electrol
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INTRODUCTION 317 In various operati
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EXPERIMENTAL 0% 10 % a b 60 % a b a
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EXPERIMENTAL 381 caused by the coun
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CONCLUSION 383 c t r ’r; I I"
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APPENDICES
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Appendix A Simplified model of movi
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PROCEDURE OF COMPUTATION A.3. PROCE
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EXPERIMENTAL 39 1 TABLE A1 THEORETI
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DISCUSSION E I I Fig.A2. Graphical
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Appendix B Diameter of the narrow-b
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Appendix C Literature 1897-1966 F.
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LITERATURE 399 B.P. Konstantinov an
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LITERATURE 401 1971 L. Arlinger, Is
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LITERATURE 403 1973 L. Arlinger and
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LITERATURE 405 A. Chrambach and J.S
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LITERATURE 407 M. Coxon and M.J. Bi
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Symbols and abbreviations SYMBOLS A
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SYMBOLS AND ABBREVIATIONS SUPERSCRI
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Subject index A Absorption meter, U
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SUBJECT INDEX 41 5 Detection limit
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SUBJECT INDEX 41 7 --_ , separation
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