Chromatography Theory

Автор(ы):Cazes J., Scott R.P.W.
Год изд.:2002
Описание: This book provides the basic theory of gas and liquid chromatography together with the foundations of thin layer chromatography. The thermodynamic and dynamic principles of chromatographic retention are considered in detail and the kinetic processes that lead to band dispersion are quantitatively developed for all three major chromatographic techniques. The factors effecting the efficacy of preparative chromatography are reviewed and a discourse on moving bed and simulated moving bed chromatography is included. In addition, the column design and the design of chromatographic equipment are also discussed. The book has been written in such a way that the mathematical skills required to -understand the arguments are reduced to a minimum. Although, the algebra is occasionally lengthy, the contents of this book will be easily understood by undergraduate scientists who have taken basic courses in algebra and calculus. This book is directed to analysts who utilize chromatographic techniques on a routine basis, scientists interested in designing chromatographic equipment, graduate students and postgraduate research fellows, and all who wish to have a fundamental understanding of the processes involved in chromatographic separation.
Chromatography Theory — обложка книги. Обложка книги.
Part 1 The Mechanism of Retention [1]
Molecular Interactions, the Thermodynamics of Distribution, the Plate Theory, and Extensions of the Plate Theory
  Chapter 1 Introduction to Chromatography Theory [3]
    Brief History of Chromatography The Development Process [7]
      Displacement Development [7]
      Frontal Analysis [8]
      Elution Development [9]
      Elution Development in Thin Layer Chromatography [12]
    Chromatographic Terminology [14]
    Synopsis [16]
    References [17]
  Chapter 2 The Control of Chromatographic Retention and Selectivity (The Plate Theory) [19]
    The Plate Theory [20]
    The Retention Volume of a Solute [24]
    The Conditions for Chromatographic Separation [25]
      The Capacity Ratio of a Solute [26]
      The Separation Ratio (Selectivity) of a Solute [27]
    The Compressibility of the Mobile Phase [28]
    The Column Dead Volume [34]
      Chromatographic Dead Volumes [38]
      Experimental Examination of Dead Volume Measurement [39]
    Synopsis [45]
    References [45]
  Chapter 3 The Distribution Coefficient and Its Control of Retention Solute [47]
    The Thermodynamic Treatment of Solute Distribution in Chromatography [47]
    The Distribution of Standard Free Energy [54]
    Thermodynamic Analysis of Some Homologous Series [54]
    Molecular Interactions and their Influence on the Magnitude of the Distribution Coefficient (K) [62]
    Molecular Interactions [63]
    Dispersion Forces [63]
    Polar Forces [65]
    Dipole-Dipole Interactions [66]
      Dipole-Induced-Dipole Interactions [67]
      Ionic Forces [69]
      Hydrophobic and Hydrophilic Interactions [71]
    The Distribution of Standard Free Energy Between Different Types of Molecular Interactions [75]
      The Concept of Complex Formation [77]
    Applied Thermodynamics [80]
    Synopsis [83]
    References [85]
  Chapter 4 The Theory of Mixed Phases in Chromatography [87]
    Introduction [87]
    Effect of Low Concentrations of Moderator [88]
      Langmuir's Adsorption Isotherm for a Single Layer [88]
      Effect of Bonding Characteristics [92]
      Langmuir's Adsorption Isotherm for a Double Layer [93]
      Mono-layer Adsorption [94]
      Bi-layer Adsorption [95]
    Interactive Mechanisms with a Stationary Phase Surface in LC [98]
      Interactions of a Solute with a Stationary Phase Surface [99]
      Experimental Support for the Sorption and Displacement Processes [102]
    High Concentrations of Moderator [106]
    Mixed Mobile Phases in LC mixed solvents [109]
      Ternary Mixtures [115]
    The Combined Effect of Temperature and Solvent Composition on Solute Retention [118]
    Validation of Temperature/Solvent-Composition Independence [123]
    Aqueous Solvent Mixtures [124]
    The Thermodynamic Properties of Water/Methanol Association [133]
    Solute Interactions with Associated Solvents [135]
      General Comments [139]
    Synopsis [140]
    References [142]
  Chapter 5 Programming Techniques [143]
    Flow Programming [144]
      Flow Programming with a Compressible Mobile Phase [146]
    Temperature Programming [149]
    Gradient Elution or Solvent Programming [157]
    Synopsis [163]
    References [164]
Chapter 6 Extensions of the Plate Theory [165]
    The Gaussian Form of the Elution Equation [165]
    Retention Measurements on Closely Eluting Peaks [167]
    Quantitative Analysis from Retention Measurements [171]
    Peak Asymmetry [175]
    Column Efficiency [179]
    The Position of the Points of Inflection [182]
    Resolving Power of a Column [183]
    Effective Plate Number [187]
    Elution Curve of a Finite Charge [190]
    Summation of Variances [193]
    The Maximum Sample Volume that Can Be Placed on a Chromatographic Column [194]
    Vacancy Chromatography [195]
    The Peak Capacity of a Chromatographic Column [202]
    Temperature Changes During the Passage of a Solute through a Theoretical Plate in Gas Chromatography [209]
    A Theoretical Treatment of the Heat of Absorption Detector [218]
    Synopsis [231]
    References [233]
Part 2 The Mechanism of Dispersion
Dispersion in Columns and Mobile Phase Conduits, the Dynamics of Chromatography, the Rate Theory and Experimental Support of the Rate Theory [235]
  Chapter 7 The Dynamics of Peak Dispersion [237]
    The Random Walk Model [240]
    The Diffusion Process [243]
    Sources of Dispersion in a Packed Column [245]
      Dispersion from the Multi-Path Effect [245]
      Dispersion from Longitudinal Diffusion [247]
      Longitudinal Diffusion in the Stationary Phase [248]
    Dispersion Due to Resistance to Mass Transfer [250]
      Resistance to Mass Transfer in the Mobile Phase [250]
      Resistance to Mass Transfer in the Stationary Phase [251]
    Quantitative Treatment of Resistance to Mass Transfer Dispersion [252]
      Diffusion Controlled Dispersion in the Stationary Phase [254]
      Diffusion Controlled Dispersion in the Mobile Phase [255]
    Fudge Factors [257]
    Synopsis [258]
    References [259]
  Chapter 8 The Rate Theory Equations [261]
    The Giddings Equation [261]
    The Huber Equation [262]
    The Knox Equation [264]
    The Horvath and Lin Equation [265]
    The Golay Equation [266]
    Effect of Mobile Phase Compressibility on the HETP Equation for a Packed GC Column [267]
    Mobile Phase Compressibility: Its Effect on the Interpretation of Chromatographic Data in LC [273]
    Effect of Mobile Phase Compressibility on the HETP Equation for a Packed LC Column [275]
    Extensions of the HETP Equation [276]
      Packed GC Columns [278]
      Packed LC Columns [279]
      Open Tubular GC Columns [281]
    Synopsis [283]
    References [284]
  Chapter 9 Extra-column Dispersion [287]
    Dispersion Generated by Different Parts of the Chromatographic System [290]
    Dispersion Due to Sample Volume [290]
    Dispersion in Sample Valves [293]
    Dispersion in Unions and Stainless Steel Frits [294]
    Dispersion in Open Tubular Conduits [295]
    Low Dispersion Connecting Tubes [300]
      Serpentine Tubes [302]
    Dispersion in the Detector Sensor Volume [305]
      Dispersion in Detector Sensors Resulting from Newtonian Flow [305]
      Apparent Dispersion from Detector Sensor Volume [306]
    Dispersion Resulting from the Overall Detector Time Constant [310]
    Synopsis [311]
    References [312]
  Chapter 10 Experimental Validation of the Van Deemter Equation [315]
    The Accurate Measurement of Column Dispersion [316]
    The Multi-path, or (A), Term [321]
    The Longitudinal Diffusion, or (B), Term [324]
    The Optimum Velocity and the Minimum Plate Height [325]
    Dispersion Due to Resistance to the Mass Transfer of the Solute between the Two Phases [328]
    The Effect of Particle Size on the Magnitude of the Van Deemter (C) Term [329]
    The Effect of the Function of (k') on Peak Dispersion [330]
    Synopsis [333]
    References [333]
  Chapter 11 The Measurement of Solute Diffusivity and Molecular Weight [335]
    The Relationship between Dispersion in a Packed Column to Solute Molecular Weight [343]
    Synopsis [356]
    References [358]
  Chapter 12 Chromatography Column Design [359]
    The Design of Packed Columns for GC and LC [359]
    Performance Criteria [361]
      The Reduced Chromatogram [361]
    Instrument Constraints [363]
    Elective Variables [364]
    Column Specifications and Operating Conditions [365]
    Analytical Specifications [366]
    The Column Design Process for Packed Columns [367]
    The Optimum Particle Diameter [370]
      Packed GC Columns [373]
      Packed LC Columns [376]
    The Optimum Column Radius [379]
    The Optimum Flow Rate [381]
    The Minimum Solvent Consumption [382]
    Maximum Sample Volume [383]
    Synopsis [383]
    Reference [394]
  Chapter 13 Chromatography Column Design: The Design of Open Tubular Columns for GC [385]
    The Optimum Column Radius [388]
    The Minimum Length of an Open Tubular Column [390]
    Minimum Analysis Time [391]
    The Optimum Flow-Rate [391]
    Maximum Sample Volume and Maximum Extra Column Dispersion [392]
    Synopsis [393]
  Chapter 14 Chromatography Column Design: Application of the Design Equations to Packed Liquid Chromatography Columns and Open Tubular Gas Chromatography Columns [395]
    Optimized Packed Columns for LC [395]
    The Optimum Particle Diameter [396]
    The Optimum Velocity [398]
    The Minimum Plate Height [400]
    The Minimum Column Length [401]
    The Minimum Analysis Time [402]
    The Optimum Column Radius [403]
    The Optimum Flow Rate [404]
    Solvent Consumption [405]
    The Maximum Sample Volume [406]
    Gradient Elution [407]
    Optimized Open Tubular Columns for GC [409]
    The Optimum Column Radius [409]
    The Optimum Mobile Phase Velocity [411]
    The Calculation of (Hmin) [412]
    The Optimum Column Length [413]
    The Analysis Time [414]
    The Optimum Flow Rate [415]
    The Maximum Sample Volume [415]
    Synopsis [417]
    Reference [418]
  Chapter 15 Preparative Chromatography [419]
    Column Overload [419]
    Column Overload Due to Excess Sample Volume [420]
    Column Overload Due to Excess Sample Mass [427]
    The Control of Sample Size for Normal Preparative Column Operation [431]
    The Moving Bed Continuous Chromatography System [433]
    Synopsis [439]
    References [441]
  Chapter 16 Thin Layer Chromatography Theory [443]
    TLC Measurements [447]
    Resolution [449]
    Measurement of TLC Efficiency [451]
    Dispersion on a Thin Layer Plate [452]
    Synopsis [453]
    References [454]
Appendix 1 The integration of the differential equation that describes the rate of change of solute concentration within a plate to the volume flow of mobile phase through it [455]
Appendix 2 Accurate and Precise Dispersion Data for LC Columns [457]
Appendix 3 List of Symbols [463]
Author Index [467]
Subject Index [469]
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