53 relatie tussen retentietijd en

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5.5.3 Relatie tussen retentietijd en verdelingscoëfficiënt ............................................................... 103 5.5.4 Capaciteitsfactor ..................................................................................................................... 103 5.5.5 Selectiviteitsfactor .................................................................................................................. 104 *5.6 Vorm van chromatografische banden en bandverbreding .......................................................... 105 5.6.1 Vorm van chromatografische banden .................................................................................... 105 5.6.2 Methoden voor het beschrijven van de efficiëntie van een chromatografische kolom ......... 106 5.6.3 van Deemter vergelijking ....................................................................................................... 107 5.7 Resolutie (of oplossend vermogen) ............................................................................................... 108 6 Vloeistofchromatografie ............................................................................................................... 111 6.1 Inleiding ......................................................................................................................................... 111 6.2 Dunne-laagchromatografie (TLC) ................................................................................................. 111 6.2.1 Principes van TLC en plaattypes ............................................................................................ 111 6.2.2 Stapsgewijze instructies voor TLC ........................................................................................ 112 6.2.2.1 Op de TLC-plaat brengen van het staal .......................................................................... 112 6.2.2.2 Keuze van het solvent voor elutie ................................................................................... 113 6.2.2.3 Elutie van de TLC-plaat .................................................................................................. 114 6.2.2.4 Evaluatie van de ontwikkelde plaat ................................................................................ 114 6.2.2.5 Weergave van de resultaten ............................................................................................. 116 6.2.3 Preparatieve TLC .................................................................................................................... 118 6.2.4 Meervoudige elutie ................................................................................................................. 119 6.2.5 Elutie van zure en basische verbindingen .............................................................................. 119 6.2.6 Elutie van zuurgevoelige verbindingen .................................................................................. 119 6.2.7 Controle op ontbinding van verbindingen ............................................................................. 119 6.2.8 Kwantitatieve TLC ................................................................................................................. 120 6.3 Papierchromatografie ..................................................................................................................... 120 6.4 Kolomchromatografie .................................................................................................................... 123 6.4.1 Principes van kolomchromatografie ...................................................................................... 123 6.4.2 Apparatuur .............................................................................................................................. 124 6.4.3 Stationaire fasen voor adsorptie-kolomchromatografie ......................................................... 124 6.4.3.1 Silicagel ........................................................................................................................... 124 6.4.3.2 Alumina ........................................................................................................................... 125 6.4.3.3 Overige stationaire fasen ................................................................................................. 126 6.4.4 Selectie van het solvent .......................................................................................................... 126
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iv 6.4.5 Vullen van de kolom met de stationaire fase ......................................................................... 128 6.4.6 Het op de kolom brengen van het staal .................................................................................. 128 6.4.7 Elutie van de kolom ................................................................................................................ 129 6.4.8 Droge-kolomchromatografie .................................................................................................. 130 6.4.9 Flash-chromatografie .............................................................................................................. 131 7 Gaschromatografie ......................................................................................................................... 133 7.1 Principes van gaschromatografie .................................................................................................. 133 7.2. Apparatuur .................................................................................................................................... 134 7.2.1 Draaggas ................................................................................................................................. 135 7.2.2 Injectie van het staal ............................................................................................................... 136 7.2.3 Kolommen .............................................................................................................................. 137 7.2.4 Kolomoven ............................................................................................................................. 139 7.2.5. Detectors ................................................................................................................................ 140 7.2.6 Dataverwerkingssysteem ........................................................................................................ 141 7.3. Stationaire fasen voor gepakte kolommen ................................................................................... 141 7.4. Detectors ....................................................................................................................................... 146 7.4.1.Vlam-ionisatie-detector (FID) ................................................................................................ 146 7.4.2 Thermische-geleidbaarheidsdetector (TCD) .......................................................................... 148 7.4.3 Elektronenvangstdetector (ECD) ........................................................................................... 150 7.4.4 Vlamfotometrische detector (detectie van P en S) ................................................................. 151 7.4.5 Thermionische vlamdetector (TID) ........................................................................................ 151 7.4.6 Zwavelchemiluminescentie detector (detectie van zwavel) .................................................. 152 7.4.7 Foto-ionisatiedetector ............................................................................................................. 152 7.4.8 Atomaire-emissiedetector ....................................................................................................... 153 7.5. Capillaire kolom gaschromatografie ............................................................................................ 154 7.6 Kwalitatieve analyse ...................................................................................................................... 157 7.6.1. Retentietijd ............................................................................................................................. 157 7.6.2. Spiking ................................................................................................................................... 157 7.6.3. Retentie-index van Kovats .................................................................................................... 157 7.6.4 Gaschromatografie als criterium voor productzuiverheid ..................................................... 159 7.7 Kwantitatieve analyse .................................................................................................................... 159 7.7.1 Normalisatie ............................................................................................................................ 160 7.7.2 Gebruik van een inwendige standaard ................................................................................... 160 7.7.3 Gebruik van een uitwendige standaard .................................................................................. 160 7.7.4 Standaardadditie ..................................................................................................................... 161 7.8 Derivaatvorming en gaschromatografie van weinig vluchtige verbindingen .............................. 162 7.8.1 Derivaatvorming ..................................................................................................................... 162 7.8.1.1 Silylering ......................................................................................................................... 163 7.8.1.2 Acetylering ...................................................................................................................... 163 7.8.1.3 Alkylering (estervorming) ............................................................................................... 164
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v 7.8.2 Gaschromatografie van anorganische verbindingen .............................................................. 164 7.8.3 Pyrolysegaschromatografie .................................................................................................... 164 7.9 GSC ................................................................................................................................................ 164 7.9.1 Principe van GSC ................................................................................................................... 164 7.9.2 Vaste stationaire fasen: ........................................................................................................... 165 7.9.2.1 Alumina ........................................................................................................................... 165 7.9.2.2 Actieve kool ..................................................................................................................... 166 7.9.2.3 Zeolieten .......................................................................................................................... 166 7.9.2.4 Silicagel ........................................................................................................................... 166 7.9.2.5 Microporeuze polymeren ................................................................................................ 166 7.9.3 Toepassingen van GSC ........................................................................................................... 167 *7.10 Gekoppelde technieken in gaschromatografie .......................................................................... 167 7.10.1 Gaschromatografie-massaspectrometrie (GC-MS) ............................................................. 167 7.10.1.1 GC-MS interfaces .......................................................................................................... 168 7.10.1.2 Ionisatie van het staal .................................................................................................... 169 7.10.1.3 Types van massa-analysetoestellen ............................................................................... 169 7.10.1.4 Uitvoeringswijzen van GC-MS ..................................................................................... 171 7.10.2 Gaschromatografie-infraroodspectroscopie (GC-IR) .......................................................... 172 7.10.3 Gecombineerde GC-MS-IR
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