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Summary - Methoden in het biofarmaceutisch onderzoek: algemene analyse
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samenvatting algemene analyse
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Inhoud0 Hoofdstuk 0: chemische analyse......................................................................................................... 7
0.1 Vraagstelling:................................................................................................................................ 7
0.2 Gepaste analytische procedures selecteren.................................................................................7
0.3 Staalname..................................................................................................................................... 7
0.4 Staalvoorbereiding........................................................................................................................ 7
0.5 analyse......................................................................................................................................... 8
0.6 interpreteren van resultaten ‘rapporteren’.....................................................................................8
0.7 conclusies trekken........................................................................................................................ 8
1 Hoofdstuk 1: metingen......................................................................................................................... 8
1.1 Inleiding........................................................................................................................................ 8
1.2 SI eenheden................................................................................................................................. 8
1.3 Prefixen......................................................................................................................................... 8
1.4 Conversie van eenheden.............................................................................................................. 9
1.5 Chemische concentraties.............................................................................................................. 9
1.6 Bereiding van oplossingen met een bepaalde molariteit.............................................................10
1.7 Verdunning van oplossingen....................................................................................................... 10
1.8 Oplossingen en stoechiometrie................................................................................................... 10
2 Hoofdstuk 2: Instrumentarium............................................................................................................ 10
2.1 Veiligheid.................................................................................................................................... 10
2.2 Pictogrammen en gevaarsymbolen: zie cursus..........................................................................11
2.3 Afval............................................................................................................................................ 11
2.4 Laboboek.................................................................................................................................... 11
2.5 Analytische balans...................................................................................................................... 11
2.5.1 Mechanische analytische balans......................................................................................... 11
2.5.2 Elektronische analytische balans......................................................................................... 11
2.6 Afwegen praktisch...................................................................................................................... 12
2.7 Ijking van een balans.................................................................................................................. 12
2.8 Buoyancy (=opwaartse kracht als we praten over balansen)......................................................12
2.9 Buretten (=glazen buis met verdelingen)....................................................................................12
2.10 Maatkolven............................................................................................................................... 12
2.11 Pipetten..................................................................................................................................... 13
2.12 Nauwkeurigheid - Precisie........................................................................................................ 13
2.13 Microliterspuit (Hamilton spuit).................................................................................................. 13
2.14 Calibratie van volumetrisch glaswerk........................................................................................ 13
2.15 Gravimetrische analyse............................................................................................................ 13
2.16 Drogen...................................................................................................................................... 13
3 Hoofdstuk 3: Verwerking analyseresultaten.......................................................................................13
3.1 Inleiding...................................................................................................................................... 13
, 3.2 Gauss of normaalverdeling......................................................................................................... 14
3.3 Gemiddelde................................................................................................................................ 14
3.4 Standaardafwijking of standaarddeviatie (minstens 3 waarden !!!).............................................14
3.5 Gemiddelde en standaardafwijking............................................................................................. 14
3.6 Grubbs-test................................................................................................................................. 14
4 Hoofdstuk 4: Foutenleer.................................................................................................................... 15
4.1 Experimentele fout...................................................................................................................... 15
4.2 Beduidende cijfers en berekeningen........................................................................................... 15
4.2.1 Optellen en aftrekken........................................................................................................... 15
4.2.2 vermenigvuldigen en delen.................................................................................................. 15
4.2.3 Logaritmen en antilogaritmen............................................................................................... 15
4.3 Soorten fouten............................................................................................................................ 16
4.3.1 Systematische fout............................................................................................................... 16
4.3.2 Toevallige fout...................................................................................................................... 16
4.4 Hoe sprijding uitdrukken?........................................................................................................... 16
4.5 Hoe fout uitdrukken..................................................................................................................... 16
4.6 Propagatie van toevallige fouten................................................................................................. 16
4.6.1 Optellen en aftrekken........................................................................................................... 16
4.6.2 Vermenigvuldigen en delen................................................................................................. 16
4.6.3 Gemengde bewerkingen...................................................................................................... 17
4.6.4 Exponenten.......................................................................................................................... 17
4.6.5 Logaritmen........................................................................................................................... 17
4.6.6 Antilogaritmen...................................................................................................................... 17
4.6.7 Beduidende cijfers in de praktijk.......................................................................................... 17
4.7 Propagatie van systematische fouten......................................................................................... 17
5 Hoofdstuk 5: chemisch evenwicht...................................................................................................... 17
5.1 De evenwichtsconstante............................................................................................................. 17
5.1.1 Evenwichtsconstanten manipuleren.....................................................................................18
5.2 Evenwicht en thermodynamica................................................................................................... 18
5.2.1 Enthalpie.............................................................................................................................. 18
5.2.2 Entropie............................................................................................................................... 18
5.2.3 Vrije energie......................................................................................................................... 18
5.2.4 Wet van Le Chatelier........................................................................................................... 18
5.3 Oplosbaarheidsproduct (Ksp)....................................................................................................... 18
5.3.1 Het gelijk-ion effect.............................................................................................................. 18
5.3.2 Scheiding door neerslag...................................................................................................... 19
5.4 Vorming van complexen............................................................................................................. 19
5.4.1 Lewis zuren en basen.......................................................................................................... 19
5.4.2 Effect van de vorming van ionische complexen op de oplosbaarheid..................................19
5.4.3 Evenwichten in tabelvorm zijn meestal niet constant...........................................................19
, 5.5 Protische zuren en basen........................................................................................................... 19
5.5.1 Bronsted-Lowry zuren en basen.......................................................................................... 19
5.5.2 Zouten.................................................................................................................................. 19
5.5.3 Geconjugeerde zuren en basen........................................................................................... 19
5.5.4 De natuur van H+ en OH-.................................................................................................... 19
5.5.5 Autoprolyse.......................................................................................................................... 19
5.6 pH............................................................................................................................................... 20
5.6.1 Bestaat puur water?............................................................................................................. 20
5.7 Sterkte van zuren en basen........................................................................................................ 20
5.7.1 Sterke zuren en basen......................................................................................................... 20
5.7.2 Zwakke zuren en basen....................................................................................................... 20
5.7.3 Gemeenschappelijke klassen van zwakke zuren en basen.................................................20
5.7.4 Polyprotische zuren en basen.............................................................................................. 20
5.7.5 Relatie tussen Ka en Kb........................................................................................................ 20
5.7.6 Afkortingen voor organische structuren...............................................................................20
6 Titraties.............................................................................................................................................. 20
6.1 Inleiding...................................................................................................................................... 20
6.2 Titraties....................................................................................................................................... 21
6.3 Primaire standaarden.................................................................................................................. 21
6.4 Berekeningen.............................................................................................................................. 21
7 Activiteit............................................................................................................................................. 22
7.1 Inleiding...................................................................................................................................... 22
7.2 Ionische sterkte en oplosbaarheid van zouten............................................................................22
7.3 Wat is “ionische sterkte”?............................................................................................................ 22
7.4 Activiteitscoefficienten................................................................................................................. 22
7.5 Berekening van de activiteitscoefficient......................................................................................22
7.6 Hydratatie van ionen................................................................................................................... 23
7.7 Berekening van de activiteitscoefficient......................................................................................23
7.8 Invloed van de ionische sterkte, ionlading en iongrootte op gamma...........................................23
7.9 Gebruik van de activiteitscoefficient............................................................................................ 23
7.10 Iteratieve methodes.................................................................................................................. 23
7.11 De pH herbekeken.................................................................................................................... 23
7.12 activiteitscoefficienten van niet-ionische verbindingen..............................................................23
7.13 Hoge ionische sterkte............................................................................................................... 24
8 Het chemisch evenwicht: systematisch............................................................................................. 24
8.1 Inleiding...................................................................................................................................... 24
8.2 Ladingsbalans............................................................................................................................. 24
8.3 Massabalans............................................................................................................................... 24
8.4 Systematische behandeling van het evenwicht..........................................................................24
8.5 Oplosbaarheid is pH afhankelijk................................................................................................. 24
, 9 Monoprotische zuur-base evenwichten............................................................................................. 25
9.1 Inleiding...................................................................................................................................... 25
9.2 Sterke zuren en basen................................................................................................................ 25
9.3 Zwakke zuren en basen.............................................................................................................. 25
9.4 Geconjugeerde zuur-base paren................................................................................................ 26
9.5 Zwak-zuur evenwichten.............................................................................................................. 26
9.6 pH van een zwak-zuur oplossing................................................................................................ 26
9.7 Dissociatiefractie voor een zuur.................................................................................................. 26
9.8 Zwak-base evenwichten............................................................................................................. 26
9.9 Associatiefractie voor een base.................................................................................................. 26
9.10 Buffers...................................................................................................................................... 26
9.11 Praktische bereiding van een buffer.......................................................................................... 27
9.12 Europese farmacopee............................................................................................................... 27
9.13 Buffercapaciteit......................................................................................................................... 27
10 Polyprotische zuur-base evenwichten............................................................................................. 28
10.1 Inleiding.................................................................................................................................... 28
10.2 Diprotische zuren/basen........................................................................................................... 28
10.3 Zure vorm H2L+......................................................................................................................... 28
10.4 Basische vorm L-...................................................................................................................... 28
10.5 Intermediaire vorm HL.............................................................................................................. 28
10.6 Algemeen: diprotische zuren.................................................................................................... 29
10.7 Diprotische buffers.................................................................................................................... 29
10.8 Polyprotische zuren en basen................................................................................................... 29
10.9 De hoofdcomponent – monoprotische systemen......................................................................29
10.10 De hoofdcomponent – diprotische systemen..........................................................................29
10.11 De hoofdcomponent – polyprotische systemen......................................................................30
10.12 Fractionele samenstelling – monoprotische systemen............................................................30
10.13 Fractionele samenstelling – polyprotische systemen..............................................................30
10.14 Isoionisch punt........................................................................................................................ 30
10.15 Isoelektrisch punt.................................................................................................................... 31
1 Zuur-base titraties.............................................................................................................................. 31
1.1 Titratiecurve................................................................................................................................ 31
1.2 Titratie van een sterke base met een sterk zuur.........................................................................31
1.3 Titratie van een zwak zuur met een sterke base.........................................................................32
1.4 Titratie van een zwakke base met een sterk zuur.......................................................................32
1.5 Titratie van diprotische systemen............................................................................................... 33
1.6 Autotitrator.................................................................................................................................. 33
1.7 Eindpuntsbepaling: afgeleiden.................................................................................................... 33
1.8 Eindpuntsbepaling: gran plot...................................................................................................... 33
1.9 Eindpuntsbepaling: indicatoren................................................................................................... 33
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