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GESLAAGD IN 1e ZIT (17/20). Samenvatting instrumentele analyse van geneesmiddelen

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Instrumentele analyse van geneesmiddelen (J000491A)

Institution
Universiteit Gent (UGent)

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Uploaded on July 7, 2024
Number of pages 237
Written in 2023/2024
Type Summary

instrumentele
instrumentele analyse
massaspectroscopie
infraroodspectroscopie

Institution
Universiteit Gent (UGent)
Education
Farmaceutische Wetenschappen
Course
Instrumentele analyse van geneesmiddelen (J000491A)

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Inhoudsopgave
1 Deel 1: algemene inleiding ............................................................................................7
1.1 Wat is analy,sche chemie? ......................................................................................................... 7
1.2 Doeleinden & werktereinen ........................................................................................................ 7
1.3 Belangrijke aspecten ................................................................................................................... 7
1.4 Système Interna,onal d’Unités (SI-units) .................................................................................... 8
2 Deel 2............................................................................................................................9
2.1 Hoofdstuk 1: Inleiding ................................................................................................................. 9
2.1.1 spectroscopie vs spectrometrie............................................................................................................ 9
2.1.2 meetprincipe van spectroscopie/ -metrie ............................................................................................ 9
2.1.3 iden6teit v atoom/molecule................................................................................................................. 9
2.1.4 structuurbeves6ging/ opheldering..................................................................................................... 10
2.2 Hoofdstuk 2: Algemene theore,sche achtergrond van spectroscopie ........................................ 10
2.2.1 elektromagne6sche straling (EMS) ..................................................................................................... 10
2.2.1.1 Zichtbaar licht (VIS) ........................................................................................................................ 11
2.2.1.2 EMS volgens GOLFtheorie ............................................................................................................. 12
2.2.1.3 EMS volgens de KWANTENtheorie ................................................................................................ 14
2.2.1.4 Eigenschappen van EMS ................................................................................................................ 14
2.2.1.5 Interac6e EMS – materie ............................................................................................................... 18
2.2.2 atomaire spectroscopie ...................................................................................................................... 20
2.2.3 moleculaire spectroscopie.................................................................................................................. 21
2.2.3.1 Mogelijke moleculaire absorp6eprocessen: .................................................................................. 21
2.2.3.2 Algemene karakteris6eken absorp6e- / emissiespectrum: ........................................................... 21
2.3 Hoofdstuk 3: atomaire absorp,e en emissiespectroscopie/spectrometrie (AAS/AES) ................ 23
2.3.1 inleiding .............................................................................................................................................. 23
2.3.1.1 Hoe gebeurt atomisa6e? ............................................................................................................... 23
2.3.1.2 Gevoeligheid meetproces .............................................................................................................. 23
2.3.2 apparatuur.......................................................................................................................................... 24
2.3.3 analy6sch gebruik............................................................................................................................... 25
2.4 Hoofdstuk 4: UV/VIS-Spectroscopie en ﬂuorescen,e................................................................. 25
2.4.1 UV/VIS-SPECTROSCOPIE: theore6sche achtergrond .......................................................................... 25
2.4.1.1 Solventeﬀecten .............................................................................................................................. 28
2.4.1.2 Eﬀect van oplosmiddel op absorp6egolﬂengte substan6es .......................................................... 28
2.4.1.3 Polaire oplosmiddelen: dipoolmoment ......................................................................................... 28
2.4.1.4 Absorp6ewaarschijnlijkheid (‘absorp6on intesity’) ....................................................................... 30
2.4.1.5 Belangrijke begrippen .................................................................................................................... 31
2.4.2 UV-spectra belangrijke verbinding ..................................................................................................... 31
2.4.2.1 Inleiding ......................................................................................................................................... 31
2.4.2.2 Conjuga6e/ mesomerie ................................................................................................................. 31
2.4.2.3 Mesomeer eﬀect van subs6tuenten (heteroatomen & andere) ................................................... 32
2.4.2.4 Induc6eve eﬀecten door subs6tuenten (heteroatomen & andere) .............................................. 32
2.4.2.5 Induc6e naast mesomerie ............................................................................................................. 33
2.4.2.6 Samenvadng ................................................................................................................................. 33
2.4.2.7 Verbindingen met geconjugeerde C=C .......................................................................................... 33
2.4.2.8 Carbonylverbindingen >C=O .......................................................................................................... 35
2.4.2.9 Aromaten ....................................................................................................................................... 37
2.4.2.10 Gesubs6tueerde aromaten ....................................................................................................... 37
2.4.2.11 Monogesubs6tueerde benzenen .............................................................................................. 38
2.4.2.12 Digesubs6tueerde benzenen .................................................................................................... 40
2.4.2.13 Zuur/base evenwichten (speciaal geval v mesomerie) ............................................................. 42

1

, 2.4.2.14 Wisselwerkingen – besluit ........................................................................................................ 43
2.4.2.15 UV/VIS voor structuurbeves6ging/ -opheldering...................................................................... 43
2.4.3 ﬂuorescen6e & ﬂuorimetrie ............................................................................................................... 44
2.4.3.1 Inleiding ......................................................................................................................................... 44
2.4.3.2 Fluorescen6e ................................................................................................................................. 46
2.4.3.3 Klassen v ﬂuorescerende moleculen ............................................................................................. 46
2.4.3.4 Fluorescen6e – analy6sche toepassing ......................................................................................... 47
2.4.4 apparatuur.......................................................................................................................................... 48
2.4.4.1 Apparatuur voor UV/VIS (spectrometer/ colorimeter) .................................................................. 48
2.4.4.2 Fluorimeter .................................................................................................................................... 50
2.4.4.3 Absorp6ewejen ............................................................................................................................ 50
2.4.4.4 Absorp6ewejen – aﬂeiding wet van Lambert-Beer ...................................................................... 51
2.4.4.5 Fluorimetrie ................................................................................................................................... 57
2.4.4.6 Kalibra6e ........................................................................................................................................ 59
2.4.4.7 Spectrometrie – prak6sche uitvoering .......................................................................................... 63
2.4.4.8 Toepassing spectrometrie .............................................................................................................. 64
2.5 Hoofdstuk 5: infraroodspectroscopie (IR) .................................................................................. 66
2.5.1 inleiding .............................................................................................................................................. 66
2.5.2 theorie ................................................................................................................................................ 67
2.5.2.1 IR spectrum.................................................................................................................................... 67
2.5.2.2 Molecuultrillingen – wiskundige benadering ................................................................................ 68
2.5.2.3 Voorwaarden voor IR-absorp6e (selec6eregel) ............................................................................. 71
2.5.2.4 Trillingen in een molecule R-AB2 .................................................................................................... 74
2.5.2.5 Fundamentele trillingen – overzicht .............................................................................................. 74
2.5.2.6 Boventonen & combina6etonen ................................................................................................... 75
2.5.2.7 Intensiteit absorp6ebanden .......................................................................................................... 75
2.5.3 invloeden op trillingsfrequen6es........................................................................................................ 76
2.5.3.1 Massa’s van de atomen ................................................................................................................. 76
2.5.3.2 Structuur (naastliggende bindingen) ............................................................................................. 77
2.5.3.3 Bindingssterkte .............................................................................................................................. 78
2.5.3.4 Bindingskarakter (hybridisa6e) ...................................................................................................... 78
2.5.3.5 Conjuga6e (elektronendelokalisa6e) ............................................................................................. 79
2.5.3.6 Intramoleculaire H-brugvorming ................................................................................................... 79
2.5.3.7 Ladingsdelokalisa6e ....................................................................................................................... 81
2.5.3.8 Samenvadng ................................................................................................................................. 82
2.5.4 absorp6egebieden & types trillingen ................................................................................................. 82
2.5.5 IR apparatuur...................................................................................................................................... 83
2.5.5.1 Energiebron IR ............................................................................................................................... 83
2.5.5.2 Op6sch gedeelte ............................................................................................................................ 83
2.5.5.3 Detectoren ..................................................................................................................................... 84
2.5.5.4 Staalvoorbereiding......................................................................................................................... 84
2.5.6 ontleden van een IR-spectrum (!!!) .................................................................................................... 85
2.5.6.1 Stap 1 ............................................................................................................................................. 85
2.5.6.2 Stap 2 ............................................................................................................................................. 85
2.5.6.3 Stap 3 ............................................................................................................................................. 85
2.5.6.4 Stap 4 ............................................................................................................................................. 86
2.5.6.5 (stap 5) ........................................................................................................................................... 86
2.6 Hoofdstuk 6: Nucleair Magne,sche Resonan,e (NMR) Spectroscopie ....................................... 92
2.6.1 inleiding .............................................................................................................................................. 92
2.6.1.1 Eigenschappen van atoomkernen.................................................................................................. 92
2.6.1.2 Kernspin ......................................................................................................................................... 92
2.6.1.3 Eigenschap van atoomkern met spin ............................................................................................. 93
2.6.1.4 Het magne6sch moment µ ............................................................................................................ 94
2.6.1.5 karakteris6eken geselecteerde kernen .......................................................................................... 95
2.6.1.6 NMR-spectroscopie ....................................................................................................................... 95
2.6.1.7 Kern in magne6sch veld – klassiek model ..................................................................................... 95

2

, 2.6.2 CHEMISCHE VERSCHUIVING ............................................................................................................... 99
2.6.2.1 Afscherming (‘shielding’) ............................................................................................................... 99
2.6.2.2 De NMR schaal............................................................................................................................. 100
2.6.2.3 Samenvadng – δ ......................................................................................................................... 101
2.6.2.4 Dimensies voor δ ......................................................................................................................... 102
2.6.2.5 NMR spectrum............................................................................................................................. 102
2.6.2.6 NMR-spectrum – 2 opnamemanieren ......................................................................................... 104
2.6.2.7 Samenvadng ............................................................................................................................... 104
2.6.2.8 Absorp6e-intensiteit .................................................................................................................... 105
2.6.3 NMR apparatuur............................................................................................................................... 105
2.6.4 chemische equivalen6e .................................................................................................................... 105
2.6.4.1 Voorbeelden ................................................................................................................................ 106
2.6.5 factoren die d beïnvloeden ............................................................................................................... 109
2.6.5.1 Elektronega6viteit ....................................................................................................................... 109
2.6.5.2 Hybridisa6e (s-karakter vd betrokken protonen)......................................................................... 110
2.6.5.3 Waterstoqrugvorming ................................................................................................................ 111
2.6.5.4 Magne6sche anisotropie-eﬀecten ............................................................................................... 114
2.6.5.5 Conjuga6e .................................................................................................................................... 116
2.6.5.6 “long range shielding” ................................................................................................................. 117
2.6.5.7 Samenvadng ............................................................................................................................... 117
2.6.6 spin-spin koppeling........................................................................................................................... 119
2.6.6.1 Oorzaak (opsplitsing) ................................................................................................................... 121
2.6.6.2 Opsplitsingspatroon (‘Pascal-driehoek’) ...................................................................................... 123
2.6.6.3 Samenvadng J ............................................................................................................................. 124
2.6.6.4 Conven6e ivm opslitsingssystemen ............................................................................................. 124
2.6.6.5 Koppeling – frequente structuren ............................................................................................... 124
2.6.7 2e orde spectra ................................................................................................................................. 125
2.6.8 oefening ........................................................................................................................................... 126
1
2.6.9 H-NMR: prak6sche aspecten........................................................................................................... 127
1
2.6.10 H-NMR: oefening ............................................................................................................................ 127
2.7 Hoofdstuk 7: massaspectroscopie/ massaspectrometrie ......................................................... 128
2.7.1 inleiding ............................................................................................................................................ 128
2.7.2 massaspectrometer .......................................................................................................................... 128
2.7.2.1 Inlaatsystemen............................................................................................................................. 129
2.7.2.2 Ionenbronnen .............................................................................................................................. 129
2.7.2.3 Massaﬁlters & detectoren ........................................................................................................... 131
2.7.2.4 Detectoren ................................................................................................................................... 134
2.7.2.5 Scan-modus ................................................................................................................................. 134
2.7.2.6 SIM-modus .................................................................................................................................. 135
2.7.2.7 Aanwending van ‘Scan’ & ‘SIM’ ................................................................................................... 135
2.7.2.8 Terminologie ................................................................................................................................ 135
2.7.2.9 Voorbeeldspectrum benzamide .................................................................................................. 136
2.7.2.10 M+• " de ‘s2kstofregel’ ......................................................................................................... 137
2.7.2.11 Fragmenta2e benzamide ........................................................................................................ 137
2.7.2.12 Fragmentstructuren benzamide ............................................................................................. 138
2.7.2.13 Isotopen & massaspectrometrie ............................................................................................. 138
2.7.2.14 Fragmenta6e ........................................................................................................................... 143
2.7.2.15 Concept gelokaliseerde lading ................................................................................................ 143
2.7.2.16 Invloeden op fragmenta6e ..................................................................................................... 144
2.7.2.17 Fragmenta6emechanismen (algemeen) ................................................................................. 145
2.7.2.18 Samenvadng fragmenta6es ................................................................................................... 150
2.7.2.19 Verdere symbolen ................................................................................................................... 151
2.7.2.20 Alkanen ................................................................................................................................... 151
2.7.2.21 Alkylgesubs6tueerde alkanen ................................................................................................. 152
2.7.2.22 Cyclische koolwaterstoﬀen ..................................................................................................... 152
2.7.2.23 Aroma6sche koolwaterstoﬀen met zijketen ........................................................................... 153

3

, 2.7.3 massaspectrum van substan6eklassen ............................................................................................ 154
2.7.3.1 Alcoholen ..................................................................................................................................... 154
2.7.3.2 Amines ......................................................................................................................................... 155
2.7.3.3 Ethers & thioethers...................................................................................................................... 155
2.7.3.4 Aldehyden & ketonen .................................................................................................................. 156
2.7.3.5 Esters/ carbonzuren/ zuuramiden ............................................................................................... 157
2.7.3.6 Fragmenta6epatronen ................................................................................................................. 157
2.7.3.7 Massaspectrometer (MS) – prak6sche aspecten......................................................................... 158

3 Deel 3: chromatograﬁsche technieken & detec;eprincipes ........................................ 159
3.1 Hoofdstuk 1: algemeen theore,sche achtergrond van chromatograﬁe .................................... 159
3.1.1 inleiding ............................................................................................................................................ 159
3.1.2 essen6ële elementen ....................................................................................................................... 159
3.1.3 kolomchromatograﬁe ....................................................................................................................... 160
3.1.3.1 Beschrijving.................................................................................................................................. 160
3.1.3.2 Types kolomchromatograﬁe ........................................................................................................ 160
3.1.3.3 Overzicht LC – interac6emechanismen ....................................................................................... 161
3.1.4 scheidingsproces .............................................................................................................................. 161
3.1.4.1 De theorie van chromatograﬁe.................................................................................................... 161
3.1.4.2 Beschrijving van het scheidingsproces ........................................................................................ 162
3.1.4.3 Visualisa6e scheidingsproces ...................................................................................................... 162
3.1.4.4 Elementen vh chromatogram ...................................................................................................... 162
3.1.4.5 Piekkarakteris6eken..................................................................................................................... 163
3.1.4.6 Piekasymmetrie ........................................................................................................................... 163
3.1.5 reten6e ............................................................................................................................................. 164
3.1.5.1 Beschrijving reten6e .................................................................................................................... 164
3.1.5.2 Selec6viteitsfactor ....................................................................................................................... 165
3.1.5.3 Gebruik vd reten6ekarakteris6eken ............................................................................................ 166
3.1.5.4 Invloeden op reten6ekarakteris6eken......................................................................................... 166
3.1.6 piekverbreding ................................................................................................................................. 167
3.1.6.1 Beschrijving vh fenomeen ‘piekverbreding’ ................................................................................ 167
3.1.6.2 Van Deemtertheorie .................................................................................................................... 167
3.1.6.3 Schotel(platen)model .................................................................................................................. 171
3.1.6.4 Schotelgetal ................................................................................................................................. 172
3.1.7 scheidend vermogen ........................................................................................................................ 172
3.1.7.1 Resolu6e ...................................................................................................................................... 172
3.1.7.2 Samengestelde formule voor resolu6e........................................................................................ 173
3.1.8 doelstelling chromatograﬁe.............................................................................................................. 173
3.1.8.1 Eﬃciën6e ..................................................................................................................................... 173
3.1.8.2 Selec6viteit .................................................................................................................................. 174
3.1.8.3 Reten6e ....................................................................................................................................... 174
3.2 Hoofdstuk 2: gaschromatograﬁe ............................................................................................. 176
3.2.1 inleiding ............................................................................................................................................ 176
3.2.2 scheidingsprincipes (!!) .................................................................................................................... 177
3.2.2.1 Scheiding volgens dampspanning (kookpunt) ............................................................................ 177
3.2.2.2 Scheiding volgens aﬃniteit/selec2viteit ..................................................................................... 178
3.2.3 basisuitrus6ng .................................................................................................................................. 179
3.2.3.1 Essen6ële elementen .................................................................................................................. 179
3.2.4 massaspectometer ........................................................................................................................... 187
3.2.4.1 ‘scan’ & ‘SIM’ bij chromatograﬁe ................................................................................................. 187
3.2.4.2 ‘scan’-modus MS ......................................................................................................................... 188
3.2.5 temperatuurscontrole ...................................................................................................................... 191
3.2.5.1 Isotherme scheiding (GC) ............................................................................................................ 191
- Problemen: ........................................................................................................................................... 191
3.2.5.2 Temperatuursprogramma6e........................................................................................................ 192
3.2.5.3 Isotherm (1) vs temperatuursprogramma6e (2) .......................................................................... 192

4

, 3.2.6 prak6sche aspecten .......................................................................................................................... 193
3.2.6.1 Problema6sche substan6es voor GC-analyse .............................................................................. 193
3.2.7 kwalita6eve analyse ......................................................................................................................... 194
3.2.7.1 Toekennen naam aan (iden6ﬁceren van) pieken in chromatogram ............................................ 194
3.2.7.2 Reten6egrootheden .................................................................................................................... 194
3.2.8 kwan6ta6eve analyse ....................................................................................................................... 194
3.2.8.1 Externe standaardisa6e ............................................................................................................... 195
3.2.8.2 Interne standaardisa6e ................................................................................................................ 195
3.3 Deel 3: vloeistofchromatograﬁe .............................................................................................. 197
3.3.1 indleiding .......................................................................................................................................... 197
3.3.1.1 LC vs GC ....................................................................................................................................... 197
3.3.2 LC systeem ........................................................................................................................................ 197
3.3.2.1 Isocra6sch HPLC-systeem ............................................................................................................ 197
3.3.2.2 Schema HPLC-systeem ................................................................................................................. 197
3.3.2.3 Injec6eloop .................................................................................................................................. 198
3.3.2.4 Drukval over de kolom ................................................................................................................. 198
3.3.3 fysische acthergrond LC.................................................................................................................... 199
3.3.3.1 Reten6eparameters: zie theorie chromatograﬁe ........................................................................ 199
3.3.3.2 Reten6evolume VS reten6e6jd.................................................................................................... 199
3.3.3.3 LC chromatogram ........................................................................................................................ 200
3.3.4 indeling kolom-LC ............................................................................................................................. 200
3.3.5 adsorp2echromatograﬁe (LSC) = vloeistof-vaste fase chromatograﬁe ........................................... 200
3.3.5.1 Normale fase adsorp6echromatograﬁe, NP-LSC ......................................................................... 201
3.3.5.2 Omgekeerde fase chromatograﬁe (“Reversed Phase Chromatography”, RP) ............................. 207
3.3.5.3 Miniaturisa6e HPLC ..................................................................................................................... 209
3.3.6 verdelingschromatograﬁe (LLC) = vloeistof-vloeistof chromatograﬁe/ par66echromatograﬁe ...... 210
3.3.7 ionenuitwisselingschromatograﬁe (IEC) = Ion Exchange Chromatography .................................... 210
3.3.7.1 Voorwaarde voor te chromatograferen substan6es: .................................................................. 210
3.3.7.2 Sta6onaire fase ............................................................................................................................ 210
3.3.7.3 Mobiele fase ................................................................................................................................ 211
3.3.7.4 Interac2eprincipe: elektrosta6sche aantrekking (‘aﬃniteit’) ..................................................... 211
3.3.7.5 Matrices v ionenuitwisselaar....................................................................................................... 211
3.3.7.6 Indeling ionenuitwisselaars ......................................................................................................... 212
3.3.7.7 Verdelingscoëﬃciënt bij IEC (!!) ................................................................................................... 212
3.3.7.8 Evenwicht/ selec6viteit/ verdelingscoëﬃciënt ............................................................................ 213
3.3.7.9 Verdelingscoëﬃciënt/ capaciteitsfactor ...................................................................................... 213
3.3.7.10 Scheiding/ aﬃniteit/ elu6evolgorde ....................................................................................... 213
3.3.7.11 Invloed tegenion in mobiele fase op K/k’ ............................................................................... 215
3.3.7.12 IEC & elu6e zuren en basen .................................................................................................... 215
3.3.7.13 Scheiding 2 aminozuren .......................................................................................................... 215
3.3.7.14 Toepassingsgebieden IEC ........................................................................................................ 216
3.3.8 gelchromatograﬁe (SEC) = size-exclusion chromatography (!!!) ...................................................... 217
3.3.8.1 Sta6onaire fase ............................................................................................................................ 217
3.3.8.2 Mobiele fase ................................................................................................................................ 217
3.3.8.3 Voorwaarde ................................................................................................................................. 217
3.3.8.4 Scheidingsmechanisme ............................................................................................................... 218
3.3.8.5 Kalibra6e van een gel voor SEC .................................................................................................... 219
3.3.8.6 Toepassingsgebied SEC ................................................................................................................ 219
3.3.9 aﬃniteitschromatograﬁe (AC) = aﬃnity chromatography............................................................... 220
3.3.10 overzicht vloeistofchromatograﬁe .................................................................................................... 220
3.3.11 detec6e bij LC ................................................................................................................................... 221
3.3.11.1 UV/VIS-absorp6edetector ....................................................................................................... 221
3.3.11.2 Foto(diode) Array Detector (DAD) .......................................................................................... 223
3.3.11.3 Fluorescen6edetector ............................................................................................................. 223
3.3.11.4 Elektrochemische detector ..................................................................................................... 223
3.3.11.5 Doorstroomrefractometer ...................................................................................................... 223

5

, 3.3.11.6 Massaspectrometrische detector ........................................................................................... 224
3.3.12 eigenschappen v detectoren ............................................................................................................ 224
4 Deel 4: valideren van kwan;ta;eve analysemethoden .............................................. 225

6

,1 Deel 1: algemene inleiding
1.1 Wat is analy,sche chemie?
- = kwalita1eve & kwan1ta1eve karakterisa1e van stalen
• Kwalita1eve analyse = aanwezige bestanddelen in staal iden1ﬁceren (zit juiste
component erin?)
• Kwan1ta1eve analyse = gehalte/ concentra1e van 1 of meerdere substan1es in
staal doseren (juiste hoeveelheid?)

- Vaak combi vd 2
- Voor beide analysetypes: KAN noodz zijn om versch componenten aanw in staal
voorafgaandelijk te scheiden (vaak te veel componenten in staal vr kwalita1eve/
kwan1ta1eve analyse) "component waarin je geïnteresseerd bent om te analyseren
scheiden
- Analy1sche chemie: methodes om vr scheiding, iden+ﬁca+e, dosage v substan1es in
analy1sch staal

1.2 Doeleinden & werktereinen

- Elke combi tss deze 2 kolommen = mogelijk
- Empirische formule
= eenvoudigste verhouding v # elementen in molecule (vb acetylsalicylzuur: C9H804)

1.3 Belangrijke aspecten
- Representa1eve staalname " vb. representa1eve steekproef op tableYen vr analyse
- Adequate staalvoorbereiding " oa scheiding vb chromatograﬁe, extrac1e,..
- Juiste analysemethode
1) Kwan1ﬁca1elimiet
2) Accuraatheid " hoe dicht ligt resultaat bij echte resultaat?
3) Precisie " me1ngen herh => hoe dicht bij elkaar? (toevallige spreiding)
4) Monstercapaciteit " vb techniek nodig vr kleine hoeveelh/ niet elke mol even goed
meetbaar met elke spectrometrische techniek
è probleemstelling " juiste analysemethode kiezen/ juiste techniek afh v wat je moet
analyseren !!
è zie methodevalidatie

7

,1.4 Système Interna,onal d’Unités (SI-units)
- Eenheden om meetresultaten v bepaalde grootheden uit te drukken " ALTIJD !!
- Basis SI- eenheden:
Grootheid Naam Symbool

Lengte meter m
Massa kilogram kg
Tijd seconde s
Elektrische stroom ampère A
Temperatuur kelvin K
Hoeveelheid substan1e mole mol
Lich1ntensiteit candela cd
Kataly1sche hoeveelheid katal kat

- Afgeleide SI-eenheden:
• Vermenigv basiseenheid met zichzelf " vb volume (m3)
• Combi 2 of meerdere basiseenheden (vemenigv/ deling) " vb snelheid (m/s)
• Opm: strikt genomen katal ook afgeleide SI-eenheid: mol/s
• Afgeleide SI-eenheden met speciale namen
§ Hertz (Hz): 1/s
§ Newton (eenheid v kracht, N): m.kg/s2
§ Joule (eenheid v energie, J): N.m
§ Coulomb (eenheid v elektrische lading, C): A.s
§ Ohm (eenheid v elektrische weerstand, W): V/A
§ Volt (eenheid v elektrische poten1aal, V): W/A
§ WaY (eenheid v vermogen, W): J/s

- SI-preﬁxen: om decimale meervouden & submeervouden van SI-eenheden te vormen

- Niet-SI eenheden:
Grootheid Naam Symbool

Tijd minuut min = 60 s
uur h = 3600 s
Volume liter l = 10-3 m3
Massa ton t = 103 kg
Lengte angstrom Å = 10-10 m
Energie elektronvolt eV = 1.602*10-19 J
è « Comité Général des Poids et des Mesures » (CGPM)
è omzeGen in SI-eenheden !!

8

,2 Deel 2
2.1 Hoofdstuk 1: Inleiding
2.1.1 SPECTROSCOPIE VS SPECTROMETRIE
- Spectroscopie " kwalita+eve analyse
• Struuctuur/iden1teit organische substan1es beves1gen (kijken of h erin zit)
• Struct/iden11eit organische substan1es ophelderen (weet niet wat erin zit "
kijken wat erin zit)
- Spectrometrie " kwan+ta+eve analyse (= doen als je weet wat erin zit)

= gegevens uit wat je staal doet met elektromagnetische straling (EMS) " EMS (vb
infraroodlicht) uit toestel voor staal " interactie tss EMS & staal " info over welke molecule
in staal + hoeveel v molecule

2.1.2 MEETPRINCIPE VAN SPECTROSCOPIE/ -METRIE
- Wisselwerking EMS met bepaalde E-inhoud met materie (moleculen/atomen) (straling nr
molecule sturen)
- Wisselwerking: geregistreerd onder vorm v spectrum (‘vingerafdruk’/ ‘ﬁngerprint’) v
atoom/ molecule
• Je krijgt spectrum
• Spectrum anders v elke molecule/ elke molecule doet iets anders met straling "
obv spectrum: bepalen welke molecule
• Nieuwe molecule gemaakt " kijken welke molecule gemaakt
- Vb: structuurbeves1ging 2-acetoxybenzoëzuur, gesynthe1seerd vn o-hydroxybenzoëzuur
met azijnzuuranhydride

2.1.3 IDENTITEIT V ATOOM/MOLECULE
- Atoom: iden1teit eenduidig
- Molecule: iden1teit door struct bepaald (molecule = som v versch elementen)
- Organische moleculen opgebouwd uit:
• C-skelet (geraamte v molecule):
§ Verzadigde ketens: C-C
§ Onverzadigde ketens: C=C, C≡C
§ Aroma1sch skelet: vb C6H6 benzeen
§ Heterocyclisch skelet: vb C6H5N pyridine
• Func+onele groepen (gevormd door atomen/atoomgroepen die in
koolwaterstotinding 1/meer H-atomen vervangen)
§ Groepen die 1 H-atoom vervangen: vb. –OH; -COOH, -NH2; -SH; -NO2, -X
§ Groepen die 2 H-atomen aan 1 C vervangen: vb. =O; =NH
§ Groepen die 3 H-atomen aan 1 C vervangen: vb. ≡N
§ Groepen die gelijk1jdig 2 H-atomen aan 2 verschillende C-atomen
vervangen: vb. –O-, -N(H)-
" organische struct bepaalt spectrum

9

, 2.1.4 STRUCTUURBEVESTIGING/ OPHELDERING
- Molecuulspectroscopie
- Belangrijkste technieken:
1. Ultraviolet- & zichtbaar licht (UV-VIS):
• Absorp1e EMS uit UV/VIS-gebied stralingsspectrum w bestudeerd
2. Fluorescen1e:
• Emissie UV/VIS EMS na voorafgaande absorp1e v EMS uit UV- gebied v
stralingsspectrum w bestudeerd
3. Infraroodspectroscopie:
• Absorp1e EMS uit IR-gebied stralingsspectrum w bestudeerd
4. Nucleair magne1sche resonan1espectroscopie:
• Absorp1e radiogolven + magne1sch veld
5. Massaspectroscopie:
• Geen EMS, wel ionisa1e/fragmenta1e (geen EMS, wel spectroscopische techniek)

" Elke spectroscopische techniek: gebruik v versch stukje v elektromagnetisch spectrum (vb
infraroodspectroscopie gebruikt IR gebied)

- Opmerking ivm zuiverheid staal:
• Mengsel v substan1es (oa onzuiverheden) " mengspectrum " moeilijk tot
onmogelijk te interpreteren
ð Opzuivering (des1lla1e, scheiding,..) " beter spectrum
ð Belang v scheidingstechnieken!

2.2 Hoofdstuk 2: Algemene theore,sche achtergrond van spectroscopie
2.2.1 ELEKTROMAGNETISCHE STRALING (EMS)

- Zichtbaar licht maar beperkt gebied van EMS spectrum!

10

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GESLAAGD IN 1e ZIT (17/20). Samenvatting instrumentele analyse van geneesmiddelen

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