Analytical techniques Flashcards
Infrared radiation
- causes covalent bonds to vibrate
- different bonds have different absorptions
- frequency where they vibrate
Greenhouse gases
- absorb infrared radiation
- high atmospheric concentration
- long residence time
- randomly disperses energy
- have C=O, C-H, O-H
CH3+ fragment
15
CH3CH2+ fragment
29
CH2OH+ fragment
31
Molecular ion
- peak with largest m/z value
- Mr of molecule
M+1 peak
- above molecular ion
- presence of carbon13 isotope
Stationary phase
solid
liquid held by solid support
Mobile phase
moves through stationary phase
liquid or gas
Factors for chromatography separation
- extent of solubility in mobile phase
- adsorption to solid stationary phase
Thin layer chromatopgraphy
- Aluminium oxide or silicon oxide on glass plate is stationary phase
- sample spotted onto plate
- in shut container with solvent
- use iodine crystal, UV or ninhydrin to make colourless compounds visible
Rf
distance moved by solute/ distance moved by solvent
Gas chromatography
- sample vaporised and injected
- carrier gas- mobile phase (nitrogen)
- flows under pressure through column
- stationary phase- liquid or solid on solid support
- components separate as pass through column
- separately detected by signal when emerge
- retention time recorded
Retention time
time between injection of the sample and the emergence of a component from the column
Retention area
area = base x 1/2 x height
amount of component
TMS standard
1.12H equivalent and is standardised at 0ppm
2. 4C equivalent and is standardised at 0ppm
3. volatile and easy to remove
4. chemically inert and doesn’t react
5. absorbs at very high frequency- mass spec doesn’t overlap
TMS
tetramethylsilane
Si(CH3)4
NMR method
- dissolved in deuterated solvent
- add TMS as reference
- placed in strong magnetic field
- range of different radio frequencies
- different frequencies absorbed dependent on environment
D2O
- peaks for OH and NH disappear
- peaks found too wide a range - difficult to assign
Use of deuterated solvent
- doesn’t contain protons
- won’t produce extra peaks
- example- CDCl3