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Samenvatting Spectrofotometrie
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Samenvatting van het onderdeel spectrofotometrie uit het vak Instrumentele analyse 2 jaar
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INSTRUMENTELE ANALYSE 2:SPECTROFOTOMETRIE
Lector. De Bruycker Sven
Opm: 2023 - 2024
• examen gaat meer op oefeningen focussen
• blokschema’s instrumenten kunnen tekenen + beetje uitleg → GEEN detail
,INHOUD
1. UV/VIS-spectrofotometrie...................................................................................................................................................... 3
1.1 Licht als een golf............................................................................................................................................................... 3
1.2 Licht als een deeltje ......................................................................................................................................................... 3
1.3 Absorptie van licht ........................................................................................................................................................... 3
1.4 Spectrofotometrie............................................................................................................................................................ 4
1.5 Transmissie ...................................................................................................................................................................... 4
1.6 Extinctie ........................................................................................................................................................................... 4
1.7 Wet van Lambert-Beer ..................................................................................................................................................... 4
1.8 Extinctiecurve................................................................................................................................................................... 5
1.9 VIS-spectrofotometrie...................................................................................................................................................... 6
1.10 UV-spectrofotometrie .................................................................................................................................................... 6
1.11 Enkelstraal UV/VIS-spectrofotometer ............................................................................................................................ 7
1.12 Dubbelstraal UV/VIS-spectrofotometer ......................................................................................................................... 7
1.13 Meerkanaalsspectrofotmeter ........................................................................................................................................ 8
1.14 nauwkeurigeheid ........................................................................................................................................................... 9
Oefeningen ............................................................................................................................................................................ 9
2. Atomaire absorptie spectrofotometrie (AAS)....................................................................................................................... 10
2.1 Bekomen van atomen .................................................................................................................................................... 11
2.2 Instrument ..................................................................................................................................................................... 11
2.3 Meting met AAS : ijklijn .................................................................................................................................................. 14
2.4 Interferenties ................................................................................................................................................................. 14
2.5 Kookboek ....................................................................................................................................................................... 16
2.6 Toepassingen AAS .......................................................................................................................................................... 16
Oefeningen .......................................................................................................................................................................... 16
3. Fluorimetrie .......................................................................................................................................................................... 17
3.1 Inleiding ......................................................................................................................................................................... 17
3.2 Fluorescentie van een atoom......................................................................................................................................... 17
3.3 Fluorescentie van een molecuul .................................................................................................................................... 17
3.4 Absorptie en emissie ...................................................................................................................................................... 19
3.5 Fluorimetrie ................................................................................................................................................................... 19
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Moons N
, 3.6 Fluorimeter .................................................................................................................................................................... 20
3.7 Analytische werkwijze .................................................................................................................................................... 20
3.8 Kwantitatieve fluorimetrie ............................................................................................................................................. 20
3.9 Verlies van lineariteit ..................................................................................................................................................... 21
3.10 Vergelijking met UV/VIS-spectrofotometrie ................................................................................................................ 21
3.11 Toepassingen ............................................................................................................................................................... 21
4. Nefelometrie ........................................................................................................................................................................ 22
4.1 Spectrofotometrie gebaseerd op verstrooiing ............................................................................................................... 22
4.2 Golflengte keuze ............................................................................................................................................................ 23
4.3 Analytische werkwijze .................................................................................................................................................... 23
4.4 Vergelijking .................................................................................................................................................................... 23
4.5 Toepassingen ................................................................................................................................................................. 23
Oefeningen .......................................................................................................................................................................... 23
5. Atomaire emissie spectrometrie AES ................................................................................................................................... 24
5.1 Atomaire spectrofotometrie .......................................................................................................................................... 24
5.2 Definitie.......................................................................................................................................................................... 24
5.3 Instrument (blokschema) ............................................................................................................................................... 25
5.4 Vlam emissie .................................................................................................................................................................. 25
5.5 Toepassingen ................................................................................................................................................................. 26
5.6 Interferenties ................................................................................................................................................................. 27
5.7 Vergelijking AES met AAS ............................................................................................................................................... 28
6. ICP-OES ................................................................................................................................................................................. 29
6.1 Atomaire spectrofotometrie .......................................................................................................................................... 29
6.2 Inductief gekoppeld plasma ........................................................................................................................................... 29
6.3 ICP-toorts of -brander .................................................................................................................................................... 29
6.4 Detectie van emissiestraling .......................................................................................................................................... 30
6.5 ICP-OES........................................................................................................................................................................... 30
6.6 Analystische kenmerken ................................................................................................................................................ 31
6.7 Analytische kenmerken : vergelijking met AAS .............................................................................................................. 33
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, 1. UV/VIS-SPECTROFOTOMETRIE
= moleculaire spectrofotometrie
1.1 LICHT ALS EEN GOLF
Bij veel chemische analyses: absorptie of emissie van elektromagnetische straling
Elektromagnetische golven bewegen in vacuüm met de lichtsnelheid, waarbij geldt dat:
c = golflengte (m)
λ= c = lichtsnelheid = 3x108 m/s → cte
f f = frequentie (Hz)
f=
=f
1.2 LICHT ALS EEN DEELTJE
Lichtdeeltjes worden fotonen genoemd, waarbij geldt dat :
E = energie (J)
E=h×f h = constante van Planck = 6,626x10-34 J.sec
f = frequentie (Hz)
1.3 ABSORPTIE VAN LICHT
Foton nadert deeltje in grondtoestand → deeltje word geëxciteerd :
M + h . f → M*
Deeltje is hier onstabiel en valt naar originele toestand (relaxatie) waarbij overtollige E wordt overgedragen :
M* → M + warmte
Een foton met een te lagen energie zal een deeltje niet kunnen exciteren
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