Catégories : Tous - spectroscopy - elements - protons - infrared

par Imran Reedznan Il y a 8 années

498

Instrumental Analysis

Nuclear Magnetic Resonance (NMR) spectroscopy is a technique used to determine the structure of molecules by analyzing their interaction with radio waves in the presence of an external magnetic field.

Instrumental Analysis

Instrumental Analysis

AES

Generally low-viscosity soln.
Moderately expensive instrument
Flame test
light emitted through split

through prism

E-spectrum

Flame atomises metals. (converts ions -> atoms)

Each element is unique
dist. of electrons from nucleus
diff no of protons in nucleus
no. of occupied shells can be diff.

AAS

Analyte needs to be metals
Sample is sprayed into flame
Atoms being analysed that are present in the flame absorb some radiation

Amount of light absorbed indicates the quantity of the element in the original sample

Each element has a unique absorption spectrum
Elements analysed need own light source that emits the correct wavelength

Called a hallow cathode lamp

Usually measures [] of elements. i.e, [] of mercury in fish
Extremely sensitive
Very versatile, able to detect over 70 elements
Most of widely used of modern instrumental techniques

UV-Vis Spectroscopy

Low molecular mass & and it has to be an organic molecule
Mainly used for determining the [] of a substance in sample
i.e, determining the level of nutrients in water and foods
Have to select specific wavelength which strongly absorbs the comp. but not other comp. in sample
Arise when photons have enough energy to move electrons from low energy to high energy level

NMR Spectroscopy

Very expensive to buy & operate
Has to be organic molecules
Carbon-13 NMR
n+1 rule shows the num. of Carbon the actualy carbon is adjacent to
Area under the peak = ratio of C13 enviro
num of peaks = num of C13 enviro
H1 NMR
When an external magnetic field is applied to the protons spin state, they align either against (high energy) or with (low energy) the field.

The can move between energy levels by emitting or absorbing radio waves

Thus protons in diff. enviro absorb different frequencies

Peaks are split by the n+1 rule

This shows the number of protons the hydrogen is adjacent to

Area under peak = ratio of Hydrogen enviro
Chemical shifts are measured relative to (TMS). i.e, the furthest peak on the right
num of peaks = num of H enviro.
Identifies the structure of molecules using radio waves

Infrared Spectroscopy

- Moderately expensive - Requires a trained technician
Analyte has to be of organic molecules. i.e, ethanol
Most useful for qualitative analysis
Fingerprint or elucidation of structure
Can be detected due to the bonds in the molecule absorbing the infrared
Diff. bonds will absorb diff. wavelengths of infrared
Each peak represents a bond
Can identify the bond through the use of the data booklet

Chromatography

based on the principle of different rates of adsorption and desorbption to and from mobile and stationary phase
It is the separation of mixtures
TLC
Uses Retention Factor (Rf)

Poor precision & accuracy

Cheapest method of chromatography
Spots visible if coloured or under UV light
Concentrated solution is applied at base rises by capillary action
Gas Chromatography

Sample must be easily converted into a gaseous form

Sample must be volatilized without breaking down

Mobile Phase is an inert gas. i.e, Nitrogen
Most Sensitive type of chromatography. i.e, Able to detect as little as 10^-12g
Detected by heat absorption and retention time is recorded
HPLC
LIMITATIONS

Sample must be soluble in the solvent

Best to use Medium to High Molecular Mass Organic compounds as analytes
Mobile phase is a liquid. i.e, could be water+ethanol
Components detected by UV
Sensitive type of analysis. i.e, Used to check purity of drugs.