A Practical Guide to Gas Analysis by Gas Chromatography

Description

A Practical Gas Analysis by Gas Chromatography provides a detailed overview of the most important aspects of gas analysis by gas chromatography (GC) for both the novice and expert. Authors John Swinley and Piet de Coning provide the necessary information on the selection of columns and components, thus allowing the reader to assemble custom gas analysis systems for specific needs. The book brings together a wide range of disparate literature on this technique that will fill a crucial gap for those who perform different types of research, including lab operators, separation scientists, graduate students and academic researchers. This highly practical, up-to-date reference can be consulted in the lab to guide key decisions about proper setup, hardware and software selection, calibration, analysis, and more, allowing researchers to avoid the common pitfalls caused by incorrect infrastructure. 1164445938 Front-Matter_2019_A-Practical-Guide-to-Gas-Analysis-by-Gas-Chromatography A PRACTICAL GUIDE TO GAS ANALYSIS BY GAS CHROMATOGRAPHY Copyright_2019_A-Practical-Guide-to-Gas-Analysis-by-Gas-Chromatography Copyright Visual-glossary_2019_A-Practical-Guide-to-Gas-Analysis-by-Gas-Chromatography Visual glossary Introduction_2019_A-Practical-Guide-to-Gas-Analysis-by-Gas-Chromatography Introduction Chapter 1 - Overview and theory 1 - Overview and theory 1.1 Historical overview 1.1.1 Early days 1.1.2 Gas chromatography 1.1.3 Other forms of chromatography 1.1.4 Why use chromatography? 1.2 Chromatography fundamentals 1.2.1 Chemical separation 1.2.2 The mobile phase 1.2.3 Linear velocity and volumetric flow 1.2.4 The stationary phase 1.2.5 Retention time and retention factor 1.2.6 Resolution 1.2.7 Selectivity, the alpha value 1.2.8 The plate theory 1.2.9 The rate theory 1.2.9.1 Longitudinal diffusion 1.2.9.2 Slow equilibration 1.2.9.3 Flow paths 1.2.9.4 The Van Deemter equation 1.2.10 Dead volumes and unswept volumes 1.2.10.1 Feed volume 1.2.10.2 Detector volume 1.2.11 Peak symmetry 1.2.12 Overloading 1.2.13 Active sites 1.2.14 Resolution revisited 1.3 Gas laws 1.3.1 Measurement units 1.3.1.1 Units of pressure 1.3.1.2 Units of volume 1.3.1.3 Units of temperature 1.3.2 Pressure and Boyle's law 1.3.3 Temperature and Charles' law 1.3.4 Volume and Avogadro's law 1.3.5 Partial pressures and Dalton's law 1.3.6 The ideal gas law 1.3.7 Vapour pressure 1.3.8 Vapour pressure and partial pressure 1.3.9 Standard temperature and pressure (STP) References Further reading Chapter 2 - Gas analysis laboratory 2 - Gas analysis laboratory 2.1 Laboratory utilities 2.1.1 Ambient conditions 2.1.2 Ventilation 2.1.3 Electrical 2.1.4 Furniture 2.2 Getting the gases to the GC 2.2.1 Gas generators 2.2.2 Plant gas 2.2.3 Pressurised gas 2.2.4 Pressure reduction 2.2.5 Tubing 2.2.6 Fittings 2.2.7 Finally 2.3 Gases 2.3.1 Carrier gas 2.3.2 Gas standards 2.3.3 Detector gases 2.3.4 Other gases and gas lines 2.3.5 Removing gaseous impurities 2.3.6 Leak checking 2.4 Tools, accessories and spares 2.4.1 Gas handling 2.4.2 GC tools 2.4.3 General tools 2.4.4 Spares References Chapter 3 - The gas chromatograph 3 - The gas chromatograph 3.1 Gas supply 3.1.1 Manual pressure and flow control 3.1.2 Electronic flow controllers (EFCs) 3.2 Sample introduction 3.2.1 Split injection 3.2.2 Injector pneumatics 3.2.3 Splitting and quantitation 3.3 The column and column oven 3.3.1 The GC column 3.3.2 The column oven 3.3.3 Sub-ambient operation 3.4 Detectors 3.5 The data system 3.6 The ideal GC for gas analysis References Chapter 4 - Standards, calibration and samples 4 - Standards, calibration and samples 4.1 Preparation of static gas standards 4.1.1 Gravimetric method 4.1.2 Partial pressure method 4.1.3 Volumetric method 4.2 Preparation of dynamic gas standards 4.2.1 Dynamic dilution method 4.2.1.1 Mass flow controllers 4.2.1.2 Fixed restrictors 4.2.1.3 Bubble flow meters and rotameters 4.2.2 Permeation method 4.2.2.1 Making permeation tubes 4.2.2.2 Types of permeation sources 4.2.2.3 Concentration calculation 4.2.2.4 Some guidelines on the use and care of permeation sources 4.2.3 Diffusion standards 4.2.3.1 Making diffusion standards 4.2.3.2 Calibration and concentration calculation 4.2.4 Exponential dilution standards 4.3 Calibration 4.3.1 Single point calibration 4.3.2 Multi-point calibration 4.3.2.1 Calibration using dynamic dilution 4.3.2.2 Calibration using differential pressures 4.3.2.3 Calibration using static dilution 4.3.3 A good calibration References Chapter 5 - Valves 5 - Valves 5.1 Two position slider valves 5.2 Two position rotary valves 5.3 Valve handling and maintenance 5.4 Valve actuation 5.4.1 Manual actuation 5.4.2 Air actuation 5.4.3 Electric actuation 5.4.4 Micro-electric actuation 5.5 Identifying Valco™ valves 5.6 Troubleshooting valve problems 5.6.1 Internal leaks 5.6.2 Actuator problems 5.6.2.1 Air actuators 5.6.2.2 Electric actuators 5.7 Diaphragm valves 5.8 Purge housings 5.9 Multi-position valves 5.9.1 SD or dead ended valves 5.9.2 SC or common outlet valves 5.9.3 SF or flow-through valves 5.9.4 ST or trapping valves 5.9.5 STF or trapping, flow-through valves 5.10 Multi-position valve actuators 5.10.1 Manual actuators 5.10.2 Air actuators 5.10.3 Electric actuators 5.10.4 Micro-electric actuators 5.11 Mounting 5.12 Utilising timed events 5.13 Troubleshooting stream selector valves 5.14 Dean's switches References Chapter 6 - Sampling and sample introduction 6 - Sampling and sample introduction 6.1 Sampling 6.2 Sampling vessels 6.2.1 Sampling bags 6.2.2 Glass bulbs 6.2.3 Gas tight syringes 6.2.4 Canisters 6.2.5 High pressure sample cylinders 6.2.6 Other gas sample containers 6.3 Sample introduction 6.3.1 Static versus dynamic sampling 6.3.2 Syringe injection 6.3.3 Valve injection 6.3.3.1 The sample loop 6.3.3.2 The sample inlet 6.3.3.3 At-line sample inlets 6.3.3.4 Inlet valve configurations 6.3.4 Liquefied gas sample injection 6.4 Practical problem solving 6.5 Volatile organics in gas 6.5.1 Static headspace 6.5.2 Thermal desorption 6.5.3 Dynamic headspace 6.5.4 Purge-and-trap 6.5.5 Operation 6.5.6 Splitless injection 6.5.7 Programmed temperature vaporisation 6.5.8 Stacked injection 6.6 Sample excess References Chapter 7 - GC columns for gas analysis 7 - GC columns for gas analysis 7.1 Column types 7.1.1 Packed columns 7.1.2 Micro-packed columns 7.1.3 Capillary 7.1.3.1 SCOT 7.1.3.2 PLOT 7.1.3.3 WCOT 7.2 Dimensions 7.2.1 Column length 7.2.2 Internal diameter 7.2.3 Film thickness 7.2.4 Supports 7.3 Materials 7.3.1 Glass 7.3.2 Fused silica 7.3.3 Stainless and deactivated stainless steel 7.3.4 Other column materials 7.4 Column handling 7.4.1 Cutting 7.4.2 Coiling 7.4.3 Installing 7.4.3.1 Connecting fused silica columns directly on to valves 7.4.4 Temperature 7.4.5 Conditioning the column 7.5 Stationary phases 7.5.1 Molecular sieves 7.5.1.1 Aluminium silicate 7.5.1.2 Carbon molecular sieves 7.5.2 Alumina 7.5.3 Porous polymer packed columns 7.5.4 Porous polymer PLOT columns 7.5.4.1 PLOT Q 7.5.4.2 PLOT S 7.5.4.3 PLOT QS 7.5.4.4 PLOT U 7.5.5 Silica gel 7.5.6 Solid phases 7.5.6.1 Kel-F 7.5.6.2 Durapak® 7.5.6.3 Carbopack B 7.5.7 Liquid phases 7.5.7.1 PDMS 7.5.7.2 Krytox™ 7.6 Phase ratio 7.7 Column selection and care References Chapter 8 - GC detectors 8 - GC detectors 8.1 General properties of detectors 8.2 Thermal conductivity detector (TCD) 8.2.1 Principle of operation 8.2.2 Operation 8.2.3 Precautions 8.2.4 Make-up 8.2.5 Detector temperature 8.2.6 Troubleshooting 8.3 Pulsed discharge helium ionisation detector (PDHID) 8.3.1 Principle of operation 8.3.2 Precautions 8.3.3 Make-up 8.3.4 Detector temperature 8.3.5 Column installation 8.3.6 Troubleshooting 8.4 Flame ionisation detector (FID) 8.4.1 Principle of operation 8.4.2 Operation 8.4.3 Precautions 8.4.4 Make-up 8.4.5 Detector temperature 8.4.6 Troubleshooting 8.5 The methaniser FID 8.5.1 Operation 8.5.2 Precautions 8.5.3 Make-up 8.5.4 Detector temperature 8.5.5 Troubleshooting 8.6 Flame photometric detector (FPD) 8.6.1 Operation 8.6.2 Precautions 8.6.3 Make-up 8.6.4 Detector temperature 8.7 Pulsed flame photometric detector (PFPD) 8.7.1 Operation 8.7.2 Precautions 8.8 Electron capture detector (ECD) 8.8.1 Operation 8.8.2 Precautions 8.8.3 Make-up 8.8.4 Detector temperature 8.8.5 Troubleshooting 8.9 Atomic emission detector (AED) 8.10 Sulphur chemiluminescence detector (SCD) 8.11 Nitrogen chemiluminescence detector (NCD) 8.12 Photoionisation detector (PID) 8.13 Mass spectrometer (MS) 8.13.1 Principle of operation 8.13.2 Operation 8.14 Differential mobility detector (DMD) 8.15 Fourier transform-infrared (FT-IR) 8.16 Detector summary References Chapter 9 - Data system and data handling 9 - Data system and data handling 9.1 Data acquisition and processing parameters 9.1.1 Analogue to digital conversion 9.1.2 Baseline, zero and noise 9.1.3 Range and attenuation 9.1.4 Peak identification 9.1.5 Peak integration 9.1.6 Compound identification 9.1.7 Unresolved peaks 9.1.8 Timed events 9.1.9 Using timed events 9.2 Sequence and method files 9.3 Calibration, data and results processing 9.3.1 Results processing 9.3.2 Quantitation methods 9.3.2.1 Area percent 9.3.2.2 External standard 9.3.2.3 Internal standards 9.3.2.4 Standard addition 9.4 Validation of results and measurement uncertainty References Chapter 10 - Multidimensional gas analysis 10 - Multidimensional gas analysis 10.1 Introduction 10.2 Backflush-to-vent or detector 10.2.1 Principle of operation 10.2.2 Typical applications 10.2.3 Backflush-to-detector 10.2.4 Backflush time and flow 10.3 Heart cutting 10.3.1 Principle of operation 10.3.2 Typical application 10.3.3 Heart cut to column or detector 10.3.4 Column switching with a Deans switch 10.4 Series bypass 10.4.1 Principle of operation 10.4.2 Typical application 10.5 Column sequence reversal 10.5.1 Principle of operation 10.5.2 Typical application 10.6 Practical guidelines 10.7 The Micro-GC 10.8 Comprehensive two dimensional GC×GC References