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Samenvatting Instrumentele analyse

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  • January 17, 2023
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  • 2022/2023
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By: elbsalma • 8 months ago

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SAMENVATTING INSTRUMENTELE
ANALYSE
spectrochemie....................................................................................................................5
Mogelijke vragen...........................................................................................................................5
Inleiding.........................................................................................................................................5

H1. UV-vis spectrofotometrie..............................................................................................5
Wet van lambert beer....................................................................................................................5
Onderdelen apparatuur.................................................................................................................7
stralingsbron......................................................................................................................................................7
golflengteselector..............................................................................................................................................8
filters.............................................................................................................................................................9
Monochromators..........................................................................................................................................9
cuvetten...........................................................................................................................................................11
stralingsdetectie..............................................................................................................................................11
fotoomultiplicatorbuis................................................................................................................................11
siliciumfotodiode.........................................................................................................................................12

Instrumenteel ontwerp................................................................................................................14
Visuele/vergelijkende colorimetrie.................................................................................................................14
spectrofotometer...........................................................................................................................................15
fototrode.........................................................................................................................................................15

Recente ontwikkelingen in de spectrofotometrie: DATA MAnipulatie.........................................15
Toepassingen van UV-VIS absorptiemetingen..............................................................................17
Kwalitatief........................................................................................................................................................17
kwantitatief.....................................................................................................................................................17

Nefelometrie en turbidimetrie.....................................................................................................18

H2. IR spectrofotometrie...................................................................................................19
theorie.........................................................................................................................................19
Onderdelen apparatuur...............................................................................................................19
Toepassingen...............................................................................................................................21

H3: Atomaire absorptie spectrometrie.............................................................................21
inleiding.......................................................................................................................................21
Onderdelen apparatuur...............................................................................................................22
Holle kathode lamp.........................................................................................................................................22
Elektrodeloze ontladingslamp (EDL)...............................................................................................................23
Atoomcel.........................................................................................................................................................23
Vlam AAS.........................................................................................................................................................24
Grafietoven......................................................................................................................................................24


1

, toepassingen................................................................................................................................24

H4. Vlamfotometrie (AES).................................................................................................25
AES theorie..................................................................................................................................25
onderdelen..................................................................................................................................25
Vernevelen......................................................................................................................................................25
Atomiseren – exciteren...................................................................................................................................26
Isoleren spectraallijn.......................................................................................................................................26
Lichtmeting en weergave signaal....................................................................................................................26

Vlamfotometer storingen.............................................................................................................26
Zelfabsoptie.....................................................................................................................................................26
Opzuigsnelheid/ verneveling...........................................................................................................................26
Ionisatie...........................................................................................................................................................27
Fluctuaties.......................................................................................................................................................27

H5. Fluorimetrie................................................................................................................27
Fluorimetrie theorie.....................................................................................................................27
Fluorescentie opbrengst.................................................................................................................................28
Verband tss fluorescentie-intensiteit en concentratie...................................................................................28

Onderdelen apparatuur...............................................................................................................29
lichtbron..........................................................................................................................................................29
Excitatiemonochromator................................................................................................................................29
cuvet................................................................................................................................................................29
Fluorescentiemonochromator........................................................................................................................29
fluorescentiedetector......................................................................................................................................30

Toepassingen...............................................................................................................................30

H6. Massaspectrometrie...................................................................................................30
6.1 theorie...................................................................................................................................30
6.2 toestel....................................................................................................................................31
6.2.2 ionisatiebronnen.................................................................................................................31
elektron ionisatie (EI)......................................................................................................................................31
chemische ionisatie (CI)...................................................................................................................................32
Fast atom bombardement (FAB).....................................................................................................................32
Elektrospray ionisatie (ESI)..............................................................................................................................32
Atmosferisch druk chemische ionisatie (APCI)................................................................................................33
Matrix assisted laser desorption ionisation ( MALDI).....................................................................................33
Inductief gekoppelde plasma ( massaspectrometie) (ICP-MS).......................................................................34
de plasmatoorts..........................................................................................................................................35
De interface.................................................................................................................................................36
Het lenzen syssteem + foton stop...............................................................................................................37

6.2.3.Analysatoren- massascheiding............................................................................................37
Magnetische massaspectrometer...................................................................................................................37
Time of flight (TOF) analysator........................................................................................................................38
quadrupool......................................................................................................................................................39


2

, Tandem MS of MS-MS.....................................................................................................................................40
ionenvangst.....................................................................................................................................................40

detectie........................................................................................................................................40
orbitrap ( hoort eig bij detectie?.....................................................................................................................40
detectie............................................................................................................................................................41

fragmentatie................................................................................................................................41
Isotopenverhouding.....................................................................................................................42
Interpretatie................................................................................................................................42
Voorbeelden van massa spectra..................................................................................................42

H7. Nucleaire magnetische resonantie..............................................................................42
NMR theorie................................................................................................................................42
Magnetische resonantie..................................................................................................................................42
Chemische verschuiving..................................................................................................................................43

Spin spin koppeling......................................................................................................................43
Interpretatie spectra....................................................................................................................43

elektrochemie...................................................................................................................44
H8. Conductometrie theorie..............................................................................................44
theorie.........................................................................................................................................44
Toepassingen...............................................................................................................................45
Rechtstreekse meting vd geleidbaarheid........................................................................................................45
Conductometrische titraties...........................................................................................................................45

H9. Potentiometrie...........................................................................................................47
Verschijnselen in elektrochemische cellen...................................................................................47
Redoxreacties..................................................................................................................................................47
Galvanische cellen...........................................................................................................................................47
Elektrodepotentiaal.........................................................................................................................................48
Standaard elektrodepotentiaal.......................................................................................................................48
Elektrodepotentiaal ifv C.................................................................................................................................48

potentiometrie.............................................................................................................................50
activiteit - ionensterkte...................................................................................................................................50

Referentie elektrode....................................................................................................................51
Verzadigde calomel eletrode..........................................................................................................................51
zilver -zilverchloride elektrode........................................................................................................................51
Kwik- kwiksulfaat oplossing.............................................................................................................................51
Factoren die effectiviteit beïnvloeden............................................................................................................52

ionselectieve elektroden..............................................................................................................52
Glasmembraan selectief voor H+ (na+)...........................................................................................................52
assymetriepotentiaal...................................................................................................................................53
Ijking/ calibratie...........................................................................................................................................54
temperatuursafhankelijkheid.....................................................................................................................54

3

, selectiviteit en alkalifout.............................................................................................................................54

Glasmembraan selectief voor Na+...............................................................................................54
Vaste kristalmembraan selectief vr Cl-.........................................................................................55
Vloeistofmembraan selectief vr K+..............................................................................................55
Gasgevoelige elektrode selectief vr CO2......................................................................................55




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