De cursus omvat theoretische uitleg en de praktische toepassingen van volgende technieken:
destillatieprocessen (verschillende types), extractieprocessen (zowel op labo-schaal als
industriëel niveau) en verschillende types chromatografie. Daarnaast is er een algemeen hoofdstuk over het
opstelle...
Inleiding............................................................................................................................................................ 6
Basisbegrippen.............................................................................................................................................. 6
Destillatie – extractie .................................................................................................................................... 6
Destillatie ......................................................................................................................................................... 7
Faseovergang van een zuivere stof ................................................................................................................ 7
Grafische voorstelling zuivere stof – driedimensionale grafiek ................................................................... 8
Enkelvoudige of gewone destillatie van een binair mengsel ........................................................................... 9
Tx – diagram van een enkelvoudige destillatie (Examen Tekenen + fasen aanduiden) ............................... 10
Ideale mengsels....................................................................................................................................... 10
Soorten koelers om te destilleren ............................................................................................................ 11
Rectificerende of gefractioneerde destillatie ............................................................................................... 12
Principe Gefractioneerde destillatie......................................................................................................... 12
Tx – diagram van een Gefractioneerde destillatie (Examen tekenen + fasen aanduiden) .......................... 13
Oefening Tx – diagram Binair mengsel (p 17) ....................................................................................... 13
Werking van de recitificatiekolom (p18) (Examen: tekenen + onderdelen aanduiden en waar wordt de
vloeistof ingebracht)................................................................................................................................ 14
Toepassing - Fractioneerkolom ................................................................................................................ 15
Soorten fractioneerkolommen................................................................................................................. 15
Vacuümdestillatie ....................................................................................................................................... 16
Nomogram .............................................................................................................................................. 16
Stoomdestillatie .......................................................................................................................................... 17
Principe (Examen) ................................................................................................................................... 17
Voorbeelden van stoomdestillatie ........................................................................................................... 18
Azeotropische destillatie ............................................................................................................................. 18
Extractie ......................................................................................................................................................... 21
Principe ...................................................................................................................................................... 21
Vloeistof – vloeistof extractie (LLE) .............................................................................................................. 21
Opstelling scheitrechter vloeibaar – vloeibaar extractie ........................................................................... 22
Dwarsstroomextractie ............................................................................................................................. 22
Tegenstroomextractie ............................................................................................................................. 23
Dwarsstroomextractie versus tegenstroomextractie ................................................................................ 23
Voorwaarden voor een goede extractie ................................................................................................... 24
Apparatuur ............................................................................................................................................. 25
1
, 1) Mixer – settler ........................................................................................................................... 25
2) Extractiekolom ........................................................................................................................... 26
Vast – vloeistofextractie (SLE) ..................................................................................................................... 27
Principe ................................................................................................................................................... 27
Soxhlet – extractie................................................................................................................................... 27
Solid phase extractie (SPE) .......................................................................................................................... 28
Praktische uitvoering SPE ........................................................................................................................ 28
Selectie extractie A of b gaat zich binden (Mogelijke examenvraag) ......................................................... 28
Aselectieve extractie A en B binden (Mogelijke examenvraag) ................................................................. 29
1) Selectief wassen......................................................................................................................... 29
2) Selectieve elutie ......................................................................................................................... 29
Voordelen SPE t.o.v. Vloeibaar – vloeibaar extractie ................................................................................ 29
Soorten SPE............................................................................................................................................. 30
Belang van extractie tijdens de staalvoorbereiding ...................................................................................... 31
Chromatografie .............................................................................................................................................. 31
Scheidingsprincipe chromatografie.............................................................................................................. 32
Kolomchromatografie Versus TLC (Thin Layer Chromatografie) .................................................................... 33
Kolomchromatografie ............................................................................................................................. 33
Kolomchromatografie opstelling .......................................................................................................... 33
TLC (Thin Layer Chromatography of Dunne – laagchromatografie ............................................................ 34
Indeling volgens aard van de mobiele fase................................................................................................... 35
Indeling volgens het fysisch – chemisch proces (Kunnen uitleggen).............................................................. 35
Gebruikte terminologie ............................................................................................................................... 37
Detectie (Examen – detectielimiet en meetgrens bepalen (Altijd) ................................................................ 37
Bepaling piekoppervlak ........................................................................................................................... 39
Resolutie..................................................................................................................................................... 40
Piekbreedte – kolomefficiëntie ................................................................................................................ 40
Piekbreedte ......................................................................................................................................... 40
Kolomefficiëntie .................................................................................................................................. 41
Piekbreedte door diffusie ................................................................................................................ 42
Piekbreedte door Massatransfer ...................................................................................................... 42
Kolomselectiviteit.................................................................................................................................... 43
Staalvoorbereiding ...................................................................................................................................... 43
Gaschromatografie ......................................................................................................................................... 43
Apparatuur Gaschromatografie ................................................................................................................... 44
Mobiele fase: draaggas ............................................................................................................................... 45
Injecteren van het staal (Kunnen opsommen en uitleggen) .......................................................................... 45
2
, 3 manieren om het staal te injecteren ................................................................................................ 46
De kolom .................................................................................................................................................... 48
Type kolom (Welke type kolom + uitleggen) ............................................................................................ 48
Stationaire fase ....................................................................................................................................... 49
Pieken scheiden niet goed ....................................................................................................................... 49
Detectie ...................................................................................................................................................... 50
Massaspectrofotometer (MS) .................................................................................................................. 50
Andere detectoren (Kunnen uitleggen) .................................................................................................... 51
Een GC – methode ...................................................................................................................................... 51
HPLC (High Pressure Liquid Chromatography) ................................................................................................. 52
Apparatuur HPLC ........................................................................................................................................ 53
Mobiele fase ............................................................................................................................................... 53
Oefening – Bereken mobiele fase (1/2 de kans op het examen) ............................................................... 55
Pompsysteem ............................................................................................................................................. 56
Injectiesysteem ........................................................................................................................................... 56
Voorkolom .................................................................................................................................................. 57
Kolom ......................................................................................................................................................... 58
Normale phase en Reserved phase .......................................................................................................... 58
Detectie ...................................................................................................................................................... 59
UV/Vis detector....................................................................................................................................... 59
PDA – detector ........................................................................................................................................ 59
Fluorescentiedetector ............................................................................................................................. 60
Brekingsindexdetector of Refractieve index (RI) ....................................................................................... 60
Massaspectrofotometer (MS) .................................................................................................................. 61
HPLC – methode ......................................................................................................................................... 61
Uitsluitingschromatografie .............................................................................................................................. 62
Algemeen ................................................................................................................................................... 62
Stationaire fase ........................................................................................................................................... 63
Tabel kunnen interpreteren en uitleggen ................................................................................................. 64
Praktische uitvoering .................................................................................................................................. 65
Zwellen van gelkorrels ............................................................................................................................. 65
Verwijdering lucht ................................................................................................................................... 65
Verwijdering van kleine deeltjes .............................................................................................................. 65
Stapelen van de kolom ............................................................................................................................ 65
Onderdrukken van niet – specifieke reacties............................................................................................ 66
Labo – opstelling (Kunnen uitleggen) ................................................................................................... 66
Elutie ...................................................................................................................................................... 67
3
, Toepassingen .............................................................................................................................................. 67
Isolatie en zuivering van biomoleculen .................................................................................................... 67
Molecuulmassa bepaling ......................................................................................................................... 67
Ontzouten ............................................................................................................................................... 68
Bufferwisseling........................................................................................................................................ 68
Ionenwisselingschromatografie....................................................................................................................... 69
Algemeen ................................................................................................................................................... 69
Principe Ionenwisselingschromatografie...................................................................................................... 69
Stationaire fase ........................................................................................................................................... 69
Het dragermateriaal ................................................................................................................................ 70
Iogene groepen ....................................................................................................................................... 70
Mobiele fase ............................................................................................................................................... 71
Elutie .......................................................................................................................................................... 71
Toepassingen .............................................................................................................................................. 71
Het kiezen van kolom voor LC (Als eign (MW, wateroplosbaar) gegeven is, juiste chromatografie geven +
voorbeeld MF en SF ........................................................................................................................................ 72
Nabij infrarood spectroscopie (NIR)................................................................................................................. 73
Algemeen ................................................................................................................................................... 73
Principe ...................................................................................................................................................... 73
Opbouw NIR-spectrofotometer ............................................................................................................... 74
Toepassingen NIR........................................................................................................................................ 75
Analyse op punt stellen / routineanalyses ....................................................................................................... 75
Begrippen (Kennen en kunnen toepassen) .................................................................................................. 75
Hoe praktisch te werk gaan? ....................................................................................................................... 76
Het inbouwen van controles tijdens routine – analyses ............................................................................... 77
Bepaling van het ruw eiwitgehalte op bloem ................................................................................................... 78
Kjeldahlanalyse ........................................................................................................................................... 78
Principe Kjeldahlanalyse .......................................................................................................................... 78
Alternatieve methode Kjeldahlanalyse..................................................................................................... 78
Methode Kjeldahlanalyse ............................................................................................................................ 79
Stap 1: Destructie .................................................................................................................................... 79
Stap 2: stoomDestillatie........................................................................................................................... 80
Stap 3: Titratie......................................................................................................................................... 81
Bepaling vochtgehalte van de bloem (Officiële methode) ............................................................................ 81
Extractie en identificatie d.m.v. dunne laag chromatografie van cafeïne uit energiedrank en theebladeren ..... 81
Cafeïne ....................................................................................................................................................... 82
Extracties van cafeïne ................................................................................................................................. 82
4
The benefits of buying summaries with Stuvia:
Guaranteed quality through customer reviews
Stuvia customers have reviewed more than 700,000 summaries. This how you know that you are buying the best documents.
Quick and easy check-out
You can quickly pay through credit card or Stuvia-credit for the summaries. There is no membership needed.
Focus on what matters
Your fellow students write the study notes themselves, which is why the documents are always reliable and up-to-date. This ensures you quickly get to the core!
Frequently asked questions
What do I get when I buy this document?
You get a PDF, available immediately after your purchase. The purchased document is accessible anytime, anywhere and indefinitely through your profile.
Satisfaction guarantee: how does it work?
Our satisfaction guarantee ensures that you always find a study document that suits you well. You fill out a form, and our customer service team takes care of the rest.
Who am I buying these notes from?
Stuvia is a marketplace, so you are not buying this document from us, but from seller matissedecaluwe. Stuvia facilitates payment to the seller.
Will I be stuck with a subscription?
No, you only buy these notes for $9.09. You're not tied to anything after your purchase.
