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Preface xix Contributors xxi Acknowledgments xxvii Part One PGC fundamentals 1 1 An introduction 3 Chromatographic separation 3 The gas chromatograph 4 The basic instrument 4 The process instrument 5 The oven 7 Temperature control 7 Temperature programming 7 The sample injection valve 8 Laboratory and online practice 8 Plug injection 8 Gas sample injection 9 Liquid sample injection 9 The column 10 The separating device 10 It takes time 10 Multiple columns 11 SCI-FILE: On Column Types 12 Introduction to SCI-FILEs 12 Two kinds of column 12 Packed columns 12 Open-tubular columns 12 The detector 13 Making the measurements 13 The chromatogram 14 Knowledge Gained 18 Did you get it? 19 Self-assessment quiz: SAQ 01 19 Student evaluation test: SET 01 20 References 21 Cited 21 Figures 22 New technical terms 22 2 Peakshape 25 How columns work 25 What happens inside the column 26 How gas and liquid interact 26 Troubleshooting tips 28 How peaks form 28 Forming an equilibrium 28 The effect of movement 30 A peak appears 31 Effect of more equilibria 33 Some conclusions 34 Identical molecules - different behavior 34 All peaks are symmetrical 35 More equilibria - narrower peaks 35 More equilibria - taller peaks 35 Retention at the apex 36 More equilibria - same retention time 36 SCI-FILE: On Solubility 36 Solubility 36 Partition 36 Distribution 37 Limitations 37 Knowledge Gained 37 Did you get it? 38 Self-assessment quiz: SAQ 02 38 Student evaluation test: SET 02 38 References 40 Figures 40 Equation 41 Symbols 41 New technical terms 41 3 Separation 43 How peaks get separated 43 A more realistic explanation 43 A challenge question 46 Significance of the air peak 47 The answer 48 Measurements from chromatograms 50 A practical task 50 Typical calculations 51 Knowledge Gained 52 Did you get it? 53 Self-assessment quiz: SAQ 03 53 Student evaluation test: SET 03 53 References 55 Figures 55 Equations 55 Symbols 55 New technical terms 55 4 Peakpatterns 57 Migration rate 57 Predictable patterns in peak position 57 Space or time 57 Spatial or temporal separation 58 Predictable patterns in peak width 59 Distance or duration 59 SCI-FILE: On Chemical Names 60 Hydrocarbons 60 Shorthand notation 61 Predictable patterns in retention 61 The doubling rule 61 Challenge question 62 A process of elimination 62 Temperature programming 64 Relative retention 66 Separation and resolution 67 Resolution 67 Predictable patterns in resolution 69 Knowledge Gained 71 Did you get it? 72 Self-assessment quiz: SAQ 04 72 Student evaluation test: SET 04 72 References 74 Figures 74 Equations 74 Symbols 74 New technical terms 74 Part Two PGC analytics 77 5 Industrial gas chromatographs 79 Process analyzers 79 Introduction to process analysis 79 The measurement of quality 80 Process gas chromatographs 81 Versatile and reliable 81 PGC development 82 The value of analysis 83 Competing technologies 84 Gas chromatograph or spectrophotometer? 84 Speed of response 86 The outlook 87 The PGC analytics unit 87 Introduction 87 Carrier gas supply system 88 Sample injection system 89 Chromatographic valves 89 Column system 89 Detectors 89 Temperature-controlled ovens 90 Knowledge Gained 90 Did you get it? 91 Self-assessment quiz: SAQ 05 91 Student evaluation test: SET 05 92 References 93 Cited 93 Table 93 Figures 93 Symbol 94 New technical terms 94 6 Carrier gas system 95 Choice of carrier gas 95 Carrier gas purpose 95 Choice of carrier gas 95 Mixed carrier gases 97 Carrier gas purity 97 Analytical effect of impurities 98 Damaging effect of impurities 100 Maintenance of gas cleaners 101 Carrier gas supply system 101 Carrier gas supply line 102 Pressure regulation 103 Mechanical pressure regulators 103 Electronic pressure controllers 104 Flow regulation 104 Measuring the carrier gas flow rates 104 Setting the flow rates 105 Optimum flow rate 106 Knowledge Gained 106 Did you get it? 107 Self-assessment quiz: SAQ 06 107 Student evaluation test: SET 06 108 References 109 Cited 109 Table 110 Figures 110 Symbols 110 New technical terms 111 7 Sample injection 113 Introduction 113 Injecting gas samples 114 Gas sample volume 114 Gas sample temperature 115 Gas sample pressure 116 Injecting liquid samples 118 Less preferred 118 Vaporizing a liquid sample 118 Liquid sample volume 119 Liquid sample temperature 120 Liquid sample pressure 121 Other techniques 122 Sample splitting 122 Remote sample injection 122 Normalization 122 SCI-FILE: On Analytic Units 123 A fable 123 Constant sample size 123 Different ratio units 124 Injected quantity 124 Conversion of units 125 Knowledge Gained 126 Did you get it? 127 Self-assessment quiz: SAQ 07 127 Student evaluation test: SET 07 128 References 130 Cited 130 Tables 130 Figures 130 Symbols 130 New technical terms 131 8 Chromatographic valves 133 Valve technology 133 Evolution 133 The strange effect of competition 134 Valve types 135 Solenoid instrument valves 135 Spool or piston valves 135 Slide valves 136 Rotary valves 139 Diaphragm valves 141 Plunger valves for liquid injection 143 Other switching techniques 145 Valve leaks 146 About leaks 146 Valve leak mitigation 148 Knowledge Gained 149 Did you get it? 151 Self-assessment quiz: SAQ 08 151 Student evaluation test: SET 08 151 References 153 Cited 153 Table 154 Figures 154 New technical terms 155 9 Column systems 157 Two fundamental issues 157 The general elution problem 157 The temperature ramp solution 158 The multiple column solution 159 The choice 160 Delayed injection 161 Four types of column system 161 Recognizing the functions performed 161 Type A: A single column 162 Type B: Multiple columns, single detector 163 Type C: Multiple detectors, single injector 164 Type D: Multiple sample injectors 166 Elemental column systems 168 Useful techniques 168 Backflush column system 168 Distribution column system 170 Heartcut column system 171 Trap-and-hold column system 173 The real power 174 Endnote 175 Knowledge Gained 176 Did you get it? 177 Self-assessment quiz: SAQ 09 177 Student evaluation test: SET 09 177 References 180 Cited 180 Table 180 Figures 180 New technical terms 181 10 Detectors 183 Introduction 183 Types of detector 183 Two measured variables 183 Concentration detectors 184 Rate-of-arrival detectors 185 Multiple detectors 186 Signal capture 186 SCI-FILE: On Detectors 187 Signal noise 187 Speed of response 187 Sensitivity 188 Thermal conductivity detector 189 TCD application 189 TCD basic function 190 TCD detection principle 191 TCD thermal elements 192 TCD electrical arrangement 194 TCD electrical improvements 194 TCD performance enhancement 195 Flame ionization detector 197 FID application 197 FID detection principle 198 FID makeup gases 199 FID sensitivity 199 FID vent arrangements 200 FID methanator 200 Flame photometric detector 202 FPD application 202 FPD detection principle 202 FPD concerns 203 Other detectors 205 Electron capture detector 205 Helium ionization detector 206 Photoionization detector 207 Pulsed discharge detector 207 Knowledge Gained 210 Did you get it? 213 Self-assessment quiz: SAQ 10 213 Student evaluation test: SET 10 214 References 216 Cited 216 Tables 217 Figures 217 Equations 217 Symbols 218 New technical terms 218 11 Temperature control 221 Need for stability 221 Sample volume 221 Retention times 221 The air-bath oven 223 Heating with air purging 223 The airless oven 225 Heating without air 225 The 2008 ABB PGC1000 227 The 2014 Rosemount Danalyzer 370XA PGC 227 The 2009 Rosemount 700XA PGC 227 The 2002 Maxum Edition II 228 Direct column heating 228 Resistive heating 228 The ABB approach 229 The Teledyne Falcon approach 230 A few cautions 231 Summary of heating methods 231 PGC standardization 231 Realities of the market 231 The applications engineering conundrum 232 MEMS technology 233 The 2002 siemens MicroSAM 234 A closing thought 234 Knowledge Gained 235 Did you get it? 236 Self-assessment quiz: SAQ 11 236 Student evaluation test: SET 11 237 References 238 Cited 238 Table 239 Figures 239 New technical terms 240 Part Three PGC control 241 12 Event scheduling 243 A sequence of actions 243 Program timing 243 Autozero 245 Atmospheric referencing 245 Sample injection 245 Step stream 246 Column switching 247 Peak gating 247 Initiate a calculation 248 Data transmission 248 Alarm notifications 248 End-of-cycle 248 Event markers 248 Calendar events 248 Timing mechanisms 249 Mechanical programmers 249 Electronic timers 249 Microprocessor control 250 The program or method 250 Control of analyzer operation 250 Temperature control 251 Pressure control 251 Peak identification 251 Fixed-time gating 252 Retention time tracking 253 Knowledge Gained 254 Did you get it? 256 Self-assessment quiz: SAQ 12 256 Student evaluation test: SET 12 256 References 258 Cited 258 Figures 258 New technical terms 259 13 Data display techniques 261 The chromatogram display 261 Detector signal 261 Digitized chromatograms 262 Chromatogram autozero 263 Peak height calibration 263 Peak area calibration 264 The bargraph display 265 The paper saver 265 The trend record 266 Analog peak processing 266 Digital signal processing 267 The minicomputer story 267 The ubiquitous microprocessor 268 A regression perhaps? 269 Central maintenance station 271 Continuous analyzer controllers 271 PGC function alarms 272 Indicators 272 Alarm notifications 272 Knowledge Gained 273 Did you get it? 274 Self-assessment quiz: SAQ13 274 Student evaluation questions: SET-13 275 References 276 Cited 276 Table 277 Figures 278 New technical terms 278 14 Peak area integration 279 Digital chromatogram processing 279 Pulse frequency digitization 279 Signal noise measurement 281 Signal noise reduction 281 Quantifying the analyte peaks 283 Forced integration 284 Slope detection 285 Errors from baseline disturbances 286 Troubleshooting aids 287 Measuring overlapping peaks 287 Avoiding the problem 287 Tackling the problem 288 Perpendicular drop method 289 Don?t integrate to a valley point 290 Angular drop or allocated area 292 Tangent skim method 292 Effect of setup mistakes 293 Knowledge Gained 294 Did you get it? 296 Self-assessment quiz: SAQ 14 296 Student evaluation test: SET 14 296 References 298 Cited 298 Figures 299 New technical terms 299 15 Calibration 301 Measurement principles 301 Terminology 301 Random error 302 Systematic error 302 Uncertainty 302 Accurate calibration 304 Calibration and validation 304 Calibration methods 307 External standard method 307 Normalization 308 Calibrating a composite peak 309 Grab sample calibration 310 Internal standard method 310 Area percentage method 311 SCI-FILE: On Response Factors 312 External standard 312 Normalization 312 Internal standard 312 Area percentage 313 Knowledge Gained 313 Did you get it? 314 Self-assessment quiz: SAQ 15 314 Student evaluation test: SET 15 314 References 317 Cited 317 Figure 317 Equations 317 Symbols 318 New technical terms 318 Answers to self-assessment questions 319 Bibliography 329 Glossary 331 Index 367

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