Samenvatting scheidingsmethoden P4 jaar 1 LSC Inholland, 2020-2021
Door Julia Muskee
Inhoudsopgave
Week 1: Inleiding en LLE.......................................................................................................................... 3
1. Extraheren ................................................................................................................................... 3
1.1 LLE........................................................................................................................................ 4
1.2 Samenvattend ........................................................................................................................... 7
Week 2: LLE en SPE.................................................................................................................................. 7
1. Vloeistof-vloeistof extractie ........................................................................................................ 7
1.1 pH effecten LLE .................................................................................................................... 8
2 SPE chromatografie ................................................................................................................... 11
2.1 Typen vloeistof-vaste stof chromatografie ............................................................................. 12
2.1 SPE ..................................................................................................................................... 12
2.2 De basis stappen van SPE .................................................................................................. 12
Week 3: Chromatografie ....................................................................................................................... 14
1. Chromatogram .......................................................................................................................... 14
1.2 GLC en LLC verdelingschromatografie ............................................................................... 15
1.3 LSC; Adsorptie.................................................................................................................... 15
1.4 Het Chromatogram ............................................................................................................ 16
1.5 Schotelgetal ....................................................................................................................... 20
Week 4: Van Deemter vergelijking ........................................................................................................ 22
1. Van Deemter vergelijking .......................................................................................................... 22
1.1 A-term; Eddy diffusie ......................................................................................................... 22
1.2 B-term; Diffusie in breedterichting ................................................................................... 23
1.3 C-term; stroomsnelheid door de kolom ............................................................................ 24
1.4 Van Deemter vergelijking in grafiek .................................................................................. 24
Week 5: Gaschromatografie.................................................................................................................. 25
1. Typen gaschromatografie.......................................................................................................... 25
2. Voordelen gaschromatografie en toepassingsgebied ............................................................... 26
3. Gaschromatograaf ..................................................................................................................... 26
3.1 Injectiepoort ............................................................................................................................ 26
3.2 Gaschromatograaf Colomn oven....................................................................................... 28
3.3 De oven.............................................................................................................................. 31
, 3.4 De kolom............................................................................................................................ 32
3.5 De detector ........................................................................................................................ 34
4. Dragergas................................................................................................................................... 35
Week 6: HPLC & Massaspectrofotometrie ............................................................................................ 36
5. Gaschromatografie .................................................................................................................... 37
6. High-Performance Liquid Chromatography HPLC ......................................................................... 37
6.1 Systeem HPLC .......................................................................................................................... 38
6.2 Scheiding in HPLC .................................................................................................................... 40
6.3 HPLC Detectie spectrofotometrie ........................................................................................... 43
6. Massaspectrootometrie ............................................................................................................ 44
6.1 opbouw MS ....................................................................................................................... 44
7. Samenvatting......................................................................................................................... 47
Week 7................................................................................................................................................... 48
8. Andere typen chromatografie ................................................................................................... 48
8.1 HPLC en deze chromatografie ........................................................................................... 50
9. Ion exchange chromatografie ............................................................................................... 51
9.1 Verschillende stationaire fasen ............................................................................................... 51
,Week 1: Inleiding en LLE
Leerdoelen:
- het begrip extractie, verdelingscoëfficiënt, extractierendement, en distributiecoëfficiënt te
beschrijven en de voorwaarden hiervan voor een extractie te noemen
• Vanderwaalskrachten / London dispersie krachten; zwak (0.5-2.5 kcal/mol); altijd aanwezig;
afhankelijk van molecuulmassa / ketenlengte en oppervlak / ruimtelijke structuur
• Dipool–dipool interactie; zwak (1 kcal/mol)
Waterstofbruggen:
, 1.1 LLE
2. Welke eisen stel je aan de oplosmiddelen?
Niet mengbaar: polariteitsverschil
3. Welk oplosmiddel is ‘onder’ in de scheitrechter?
De vloeistof met de grootste dichtheid
4. Hoe verdeelt een stof zich over beide oplosmiddelen?
Er ontstaat een verdelingsevenwicht
(partitioned between phases)
Kd = verdelingscoefficient =
Kow = partitie octanol / water
Log P = 10Kow KOW = verdeling stof tussen octanol en water. Van zeer veel moleculen is de log P
bekend
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