Summary

Samenvatting Analytische chemie

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Course
Analytische Chemie (VA3734)

Institution
Katholieke Hogeschool VIVES (VIVES)

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...

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Uploaded on January 22, 2022
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Written in 2021/2022
Type Summary

analytische chemie
biotechnologie
2020 2021
roeselare
vives

Institution
Katholieke Hogeschool VIVES (VIVES)
Education
Agro-en Biotechnologie
Course
Analytische Chemie (VA3734)

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2. Summary - Organische chemie
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4. Summary - Anorganische chemie
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ANALYTISCHE CHEMIE
INHOUD

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

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