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37 Cards in this Set

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Chromatography



Describe the process of chromatography

1) Place the chromatography plate in the tank with a sample line at the bottom


2) Ensure the solvent level is below the sample line


3) Cover the tank and leave until the solvent front has reached the top of the plate


4) Remove the plate and mark the position of the solvent front

Chromatography



Name some uses of chromatography

Analysis of drugs, plastics, flavourings, foods, forensics, air samples, fuels etc

Chromatography



What are some benefits of chromatography?

Only small samples are needed


After separation, the pure components can be analysed precisely using other analytical methods.

Chromatography



What are the two types of chromatography you need to know?

Thin-layer


Gas

Chromatography



Generally describe the 'science' behind chromatography

A mobile phase sweeps a mixture over a stationary phase.


It works on the basis that different components have different AFFINITIES for stationary phases and mobile phases:


the stationary phase interacts with the components in the mixture, slowing them down. More interaction = more slowed down.


This allows different components to flow over the stationary phase at different speeds, separating them.

Chromatography



What is the state of the stationary and mobile phase in TLC?

Stationary - Solid


Mobile - Liquid

Chromatography



What is the state of the stationary and mobile phase in GC?

Stationary - Liquid/solid on solid support


Mobile - Gas

Chromatography



What does a solid stationary phase separate components by? Define.

ADSORPTION - the process by which a solid holds molecules of a gas/liquid or solute as a thin film on the surface of a solid

Chromatography



Draw diagrams to represent separation by adsorption and by relative solubility

Chromatography



What is the stationary phase in TLC?


A thin layer of an adsorbant such as silica gel (SiO2) or Alumina (Al2O3) coated on a flat, inert support - a TLC plate, often a sheet of glass/plastic.

Chromatography



What is the mobile phase in TLC?

A liquid solvent.

Chromatography



Rf = ?

Rf = Distance moved by solvent / Distance moved by solvent front

Chromatography



What can you use Rf values for?

To identify an unknown compound by comparing known Rf values.

Chromatography



What are the limitations of TLC?

- Similar compounds often have similar Rf values


- Unknown compounds will have no reference Rf to compare to


- It may be difficult to find a solvent that separates all the components in a mixture- too soluble in solvent = washed up with solvent front


little solubility = components will hardly move.


Chromatography



What is GC useful for?

To separate volatile compounds - useful for compounds with low boiling points and evaporate easily.

Chromatography



Describe the stationary and mobile phase in GC.

STATIONARY - Thin layer of liquid/solid coated inside capillary tubing which acts as an inert solid support.


Tubing (the chromatography column) is coiled so it fits in a thermostatically controlled oven.


The liquid stationary phase is often a long-chain alkane with a high boiling point.


Solid stationary phases include silicone polymers.


MOBILE PHASE - Carrier gas which moves through the column. An inert or inactive gas such as He or N.

Chromatography



Describe the process of GC.

1) Mixture is injected into the gas chromatogram, where it is vaporised.


2) Mobile carrier gas flushes the mixture through the column


3) As the mixture moves through the column, components slow down as the interact with the stationary phase coating the column. (liquid = dissolve, solid = adsorb) Greater solubility/adsorption = more slowed down


4) Components separate and each leaves the column at a different time and is detected as it leaves, a computer processes these results.

Chromatography



What is the retention time? + function

The time for a component to pass from the column inlet to the detector.



Can be used to identify an unknown substance if compared with known retention times


Chromatography



What are the limitations of GC?

- Many chemicals may have similar retention times, peak shape and detector response so GC might not identify them


- Not all substances will be separated and detected - a small amount of a substance can hide beneath another that has a higher conc and the same retention time


- Unknown compounds have no retention times for comparison

Chromatography



Describe GCMS.

GC - separates components, but can't identify them conclusively


MS - provides detailed structural info on most compounds but cannot separate them



1)Components in a mixture are first separated by GC. Retention time provides an initial identification


2) Separated components are put in a MS where they are detected


3) MS is analysed or compared with a spectral database

Chromatography



What is GCMS used for?

Forensic and drug analysis, environmental analysis, airport security and space probes.



Forensics = analysis minute particles found at a crime scene.


Environmental = Pollutants, quality of water, pesticides in food.


Airports = Explosives


Space = analyse atmosphere, material

NMR



What is the purpose of NMR?

Examining molecular structure.

NMR



What is chemical shift?

The place in an NMR specturm at which a nucleus absorbs energy

NMR



What is chemical shift measured relative to?

A reference signal from Tetramethylsilane TMS (CH3)4Si


Chemical shift = 0

NMR



What is the problem with using a solvent for NMR?

Organic solvents contain C and H which produce a peak themselves.

NMR



What is used as solvents?

Deuterated solvents are used as they do not produce a signal.

NMR - CARBON 13



In C13 NMR, what does chemical shift indicate?



The chemical environments of the carbon atoms present.


The presence of an electronegative element causes significant change in chemical shift.

NMR - CARBON 13



In C13 NMR:


a) Peaks show..?


b) Chemical shifts show..?


c) Size of peaks show..?

a) Number of different carbon environments


b) Types of carbon environments


c) nothing.

NMR- PROTON



In proton NMR:


a) Number of peaks show..?


b) Chemical shifts show..?


c) Size of peaks show..?


d) Splitting shows..?

a) Number of proton environments


b) Type of proton environment


c) Relative peak area = proportions of protons in each environment


d) Information of adjacent protons


NMR- PROTON



What is the N+1 rule?

For n protons on an adjacent carbon, the number of peaks on a splitting pattern is N+1.

NMR- PROTON



In proton NMR what happens when a deuterated solvent is added?

Any peaks for OH and NH disappears because it exchanges with the H present in OH or NH.

NMR- MEDICINE



Describe MRI.

Patient is placed in a large, cylindrical electromagnet and radio waves are then sent through the body, Protons align with or against the strong magnetic field and they resonate in response to pulses of radio-frequency radiation.

NMR - MEDICINE



What are the advantages of MRI?

- Harmless


-Non-invasive


NMR - MEDICINE



What are the disadvantages of MRI?

- Some patients with ferromagnetic metal implants of pacemakers should not be subjected to MRI.

NMR - MEDICINE



What are the uses of MRI in sport?

Used to identify injuries.

Combined techniques



What is the function of mass spec?

determine molecular mass of a compound.

Combined techniques



What is the function of IR?

Gives information about the bonds present in a molecule and the likely functional groups present.