Frans_M_Everaerts_Isotachophoresis_378342.pdf

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SEPARATION OF CATIONIC SPECIES IN METHANOL 367 TABLE 16.4 OPERATIONAL SYSTEM (UNBUFFERED) SUITABLE FOR CATIONIC SEPARATIONS (MHCI) Solvent: CH,OH. Electric current (MA): Ca. 50. Purification: Methanol (95%, technical grade) was purified by running it through a column filled with a mixed-bed ion exchanger (Merck V). Electrolyte Leading Terniinating + Cation Concentration Counter ion H+ 0.01 N c1- CdZ C'. 0.01 N c1- PH - - Additive None None TABLE 16.5 OPERATIONAL SYSTEM AT pH 7.4 SUITABLE FOR CATIONIC SEPARATIONS (MKAC) Solvent: CH,OH. Electric current (MA): Ca. 50. Purification: Methanol (9576, technical grade) was purified by running it through a column filled with a mixed-bed ion exchanger (Merck V). Electrolyte Leading Terminating Cation K+ Cd" Concentration 0.01 N Ca. 0.01 N Counter ion CH, COO- c1- PH 7.4 - Additive None None leading ion being W and the terminating ion Cuz+. In Fig.16.6, the isotachopherogram is given for the separation of a mixture of (CH3)41V, (C2H5)4N+, NH;, K', Na', Ca2+, Li+, Co2+, Mn2+ and Cu2+, the leading ion being H’ and the terminating ion Cd2+. 16.3.2. The operational system MKAC In this system, the leading electrolyte is potassium acetate in methanol adjusted to a pH of 7.4 by adding acetic acid. The pH is measured with a glass electrode and a calomel electrodel filled with an aqueous saturated solution of potassium chloride, as a reference electrode; The terminator used is cadmium chloride in methanol. There are large differ- ences in clornparison with the step heights of the cations in the system MHC1, particularly
368 SEPARATIONS IN NON-AQUEOUS SYSTEMS TABLE 16.6 OPERATIONAL SYSTEM AT pH 6.9 SUITABLE FOR CATIONIC SEPARATIONS (MTMAAC) Solvent : CH OH. Electric current (PA): Ca. 50. Purification: Methanol (95%, technical grade) was purified by running it through a column filled with a mixed-bed ion exchanger (Merck V). Electrolyte Leading Tcrminating Cation (CHJ4 N+ Cd” Concentration 0.01 N Ca. 0.01 N Counter ion CH, COO- cl- PH 6.9 - Additive None None TABLE 16.7 QUALITATIVE INFORMATION (STEP HEIGHTS) OF SOME CATIONIC SPECIES IN THE OPERATIONAL SYSTEMS LISTED IN TABLES 16.4-16.6 The step heights (mm) refer to 0 wA. Cation H (mm) Cation H (mm) H+ K+ Na+ Llt Rb+ cs+ Ag+ NK Tris+ TI (CH3),+ (C, H, ).,+ (C, H, ),+ Guanidine+ Succinyl choline’ Imidazole’ MHCl MKAC MTMAAC 124 - 195 195 222 230 25 7 270 180 - 168 - - 1031 179 - 292 321 - 218 154 151 170 177 265 260 192 203 209 191 176 599 *n.s.m. = not sufficiently mobile. - 198 230 260 188 173 193 317 150 186 250 198 184 NiZ+ MgZ+ Zn2+ PbZ+ BaZ* Caz+ CdZi co2+ cuz+ Mn2+ Fez+ Fe3+ A13+ Cr3+ Ce3+ La3+ MHCl MKAC MTMAAC 26 2 240 n.s.m.* n.s.m. 232 24 1 628 272 383 296 390 340 256 290 310 330 510 397 821 946 335 425 1025 497 n.s.m. 483 n.s.m. n.s.m. n.s.m. n.s.m. n.s.m. n.s.m. 560 436 960 1080 350 456 540 - 5 20 -
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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
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EXAMPLES 103 solvent, hoping that a
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EXAMPLES TABLE 5.11 STEP HEIGHTS OF
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EXAMPLES TABLE 5.12 STEP HEIGHTS OF
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Fig.5.9. Isotachopherograms of the
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EXAMPLES II 4 3 Fig.5.11. Isotachop
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REFERENCES 113 Example I. As exampl
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INSTRUMENTATION
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Chapter 6 Detection systems SUMMARY
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THERMOMETRIC RECORDING 6.1.3. Combi
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THERMOMETRIC RECORDING Potential gr
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THERMOMETRIC RECORDING /2 Fig.6.1.
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THERMOMETRIC RECORDING T t l Fig.6.
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THERMOMETRIC RECORDING 7 127 It-- I
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THERMOMETRIC RECORDING a concentrat
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HIGH-FREQUENCY CONDUCTIVITY DETECTI
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CONDUCTIVITY DETECTION 133 Fig.6.9.
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CONDUCTIVITY DETECTION 135 The d.c.
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CONDUCTIVITY DETECTION 137 Hi V 1kR
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CONDUCTIVITY DETECTION Fig.6.12. Co
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CONDUCTIVITY DETECTION Fig.6.14. Th
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CONDUCTIVITY DETECTION 143 6.4.4. T
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CONDUCTIVITY DETECTION 145 contact
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CONDUCTIVITY DETECTION 147 We can n
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CONDUCTIVITY DETECTION 149 N.Y., U.
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CONDUCTIVITY DETECTION 151 achieved
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UV ABSORPTION METER 153 -_-.- +- R
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UV ABSORPTION METER Fig.6.22. Contr
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W ABSORPTION METER r +15V -15V Mod
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W ABSORPTION METER 159 TABLE 6.4 PR
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W ABSORPTION METER 230 240 2% m zm
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to Mod (Fig 6.24) oscillator I sync
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UV ABSORPTION METER 165 dicular to
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Fig.6.31. Isotachopherograms for th
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UV ABSORPTION METER 169 50 Fig.6.33
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ADDITIVES TO THE ELECTROLYTES 171 6
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ADDITIVES TO THE ELECTROLYTES 173 e
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ADDITIVES TO THE ELECTROLYTES 175 a
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ADDITIVES TO THE ELECTROLYTES 177 o
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ADDITIVES TO THE ELECTROLYTES 179 d
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ADDITIVES TO THE ELECTROLYTES 181 T
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ADDITIVES TO THE ELECTROLYTES Fig.6
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ADDITIVES TO THE ELECTROLYTES 185 F
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ADDITIVES TO THE ELECTROLYTES 1 2 3
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ADDITIVES TO THE ELECTROLYTES 189 n
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COATING OF THE MICRO-SENSING ELECTR
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DETECTION LIMITS 193 electric drivi
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DETECTION LIMITS 195 Fig.6.48. Infl
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DETECTION LIMITS 197 TABLE 6.6 SURV
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CONCLUSION 199 average length of a
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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 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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Page 334 and 335: AMINO ACIDS Fig.13.3. Schematic dia
Page 336 and 337: AMINO ACIDS TABLE 13.6 DETERMINATIO
Page 338 and 339: SEPARATION OF PROTEINS IN AMPHOLYTE
Page 350 and 351: SEPARATION OF SMALL PEPTIDES reprod
Page 352 and 353: Chapter I4 Separation of nucleotide
Page 354 and 355: SEPARATION USING A THERMOMETRIC DET
Page 356 and 357: SEPARATION USING A THERMOMETRIC DET
Page 358 and 359: SEPARATION USING CONDUCTIVITY AND U
Page 360 and 361: SEPARATION USING CONDUCTIVITY AND U
Page 362 and 363: Chapter 15 Enzymatic reactions SUMM
Page 364 and 365: ENZYMATIC CONVERSION OF GLUCOSE (FR
Page 370 and 371: ENZYMATIC CONVERSION OF PYRUVATE 35
Page 376 and 377: Chapter 16 Separations in non-aqueo
Page 378 and 379: SEPARATION OF ANIONIC SPECIES IN ME
Page 380 and 381: SEPARATION OF CATIONIC SPECIES IN M
Page 388 and 389: EXPERIMENTS IN AQUEOUS METHANOLIC S
Page 390 and 391: Chapter I7 Counter flow of electrol
Page 392 and 393: INTRODUCTION 317 In various operati
Page 394 and 395: EXPERIMENTAL 0% 10 % a b 60 % a b a
Page 396 and 397: EXPERIMENTAL 381 caused by the coun
Page 398 and 399: CONCLUSION 383 c t r ’r; I I"
Page 400 and 401: APPENDICES
Page 402 and 403: Appendix A Simplified model of movi
Page 404 and 405: PROCEDURE OF COMPUTATION A.3. PROCE
Page 406 and 407: EXPERIMENTAL 39 1 TABLE A1 THEORETI
Page 408 and 409: DISCUSSION E I I Fig.A2. Graphical
Page 410 and 411: Appendix B Diameter of the narrow-b
Page 412 and 413: Appendix C Literature 1897-1966 F.
Page 414 and 415: LITERATURE 399 B.P. Konstantinov an
Page 416 and 417: LITERATURE 401 1971 L. Arlinger, Is
Page 418 and 419: LITERATURE 403 1973 L. Arlinger and
Page 420 and 421: LITERATURE 405 A. Chrambach and J.S
Page 422 and 423: LITERATURE 407 M. Coxon and M.J. Bi
Page 424 and 425: Symbols and abbreviations SYMBOLS A
Page 426 and 427: SYMBOLS AND ABBREVIATIONS SUPERSCRI
Page 428 and 429: Subject index A Absorption meter, U
Page 430 and 431: SUBJECT INDEX 41 5 Detection limit
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SUBJECT INDEX 41 7 --_ , separation
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