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Francis Rouessac
Chemical Analysis
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Table of Contents
List of Tables
List of Illustrations
Guide
Pages
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Chapter 1 General Aspects of Chromatography INTRODUCTION
Objectives
1.1 GENERAL CONCEPTS OF ANALYTICAL CHROMATOGRAPHY
1.2 THE CHROMATOGRAM
1.3 GAUSSIAN PEAKS AND REAL PEAKS
1.4 PLATE THEORY
1.5 NERNST PARTITION COEFFICIENT (
K
)
1.6 COLUMN EFFICIENCY 1.6.1 Theoretical Efficiency (Number of Theoretical Plates)
1.6.2 Number of Effective Plates (Real Efficiency)
1.6.3 Plate Height
Reduced plate height
1.7 RETENTION PARAMETERS 1.7.1 Retention Times
1.7.2 Retention Volume (or Elution Volume)
V
R
1.7.3 Hold‐up Volume (or Dead Volume)
V
M
1.7.4 Stationary Phase Volume
1.7.5 Retention (or Capacity) Factor k
An experimental approach to the retention factor
k
1.8 SEPARATION (OR SELECTIVITY) FACTOR
1.9 RESOLUTION FACTOR
1.10 INFLUENCE OF SPEED OF THE MOBILE PHASE
1.10.1 Van Deemter Equation
Packing‐related term
A
= 2λ.
d
p
Gas (mobile phase) diffusion term
B
= 2γ
D
G
Liquid (stationary phase) term
C
=
C
G
+
C
L
1.10.2 Golay Equation
1.10.3 Knox Equation
1.11 OPTIMIZATION OF A CHROMATOGRAPHIC ANALYSIS
1.12 CLASSIFICATION OF CHROMATOGRAPHIC TECHNIQUES
1.12.1 Liquid Chromatography (LC)
Liquid/solid chromatography (LSC)
Liquid/liquid chromatography (LLC)
Ion chromatography (IC)
Size exclusion chromatography (SEC)
Affinity chromatography
1.12.2 Gas Chromatography (GC)
Gas/solid chromatography (GSC)
Gas/liquid chromatography (GLC)
1.12.3 Supercritical Fluid Chromatography (SFC)
Quantitative Analysis by Chromatography
1.13 PRINCIPLE AND BASIC RELATIONSHIP
1.14 CHROMATOGRAPHY SOFTWARE
1.15 EXTERNAL STANDARD METHOD
1.16 INTERNAL STANDARD METHOD
1.16.1 Calculation of the Relative Response Factors
1.16.2 Chromatogram of the Sample – Calculation of the Concentrations
1.17 INTERNAL NORMALIZATION METHOD
1.17.1 Calculation of the Relative Response Factors
1.17.2 Chromatogram of the Sample – Calculation of the Concentrations
KEY POINTS OF THE CHAPTER
PROBLEMS
SOLUTIONS
Note
Chapter 2 Gas Chromatography
Objectives
2.1 COMPONENTS OF A GC INSTALLATION
2.2 CARRIER GAS AND FLOW REGULATION
2.3 INJECTION CHAMBER 2.3.1 Sample Introduction
Microsyringe and septum
Injection loops
2.3.2 Injectors
Split/splitless injector
Cold on‐column injection (COC)
Programmed temperature vaporization (PTV) injector
2.4 TEMPERATURE‐CONTROLLED OVEN
2.5 COLUMNS
2.5.1 Packed Columns
2.5.2 Capillary Columns (Open Tubular)
2.6 STATIONARY PHASES
2.6.1 Polysiloxanes
2.6.2 Polyethylene Glycols (PEG)
2.6.3 Ionic Liquids (IL)
2.6.4 Chiral Stationary Phases
Direct process
Indirect process
2.6.5 Solid Stationary Phases
2.7 MAIN DETECTORS
2.7.1 Universal or Near‐Universal Detectors Flame ionization detector (FID)
Thermal conductivity detector (TCD)
Mass spectrometry detector (MSD)
2.7.2 Selective Detectors Nitrogen phosphorus detector (NPD)
Electron capture detector (ECD)
Photo‐ionization detector (PID)
2.7.3 Detectors Providing Structural Data
2.8 OPTIMIZATION OF A SEPARATION
2.9 FAST CHROMATOGRAPHY AND MICROCHROMATOGRAPHY 2.9.1 ‘Fast’ and ‘Ultra‐Fast’ Chromatography
2.9.2 Micro Gas Chromatography
2.10 RETENTION INDEXES AND STATIONARY PHASE CONSTANTS
2.10.1 Kovats Straight‐Line Relationship
2.10.2 Kovats Retention Index
2.10.3 McReynolds Constants for Stationary Phases
KEY POINTS OF THE CHAPTER
PROBLEMS
SOLUTIONS
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