Lecture 6

Sample Preparation
 Solid Phase Extraction
(Exhaustive Extraction)

Analyte either adsorps or absorbs to a

solid support
Advantages
•Large concentrations possible
•Limited use of solvents
•Very effective clean-up technique

Disadvantages
•Time consuming
•Precision can be difficult
•Expensive
 Solid Phase Extraction - Air
(Exhaustive Extraction)

Vacuum Ambient
Environment pump
Sorbent
air

N2 in
Sorbent

Lab

Sample
 Solid Phase Extraction - Air
(Exhaustive Extraction)

Sorbents
XAD
•High surface area (290-750 m2/g)
PUF
•Polyurethane foam
TENAX
•Moderate surface area (19-30 m2/g)
•Thermally stable, appropriate for thermal
desorption
 Solid Phase Extraction - Water
(Exhaustive Extraction)

Environment Pump Sorbent Water

Water sample

Sorbent
Lab
Vacuum
manifold
Solid Phase Extraction - Water
(Exhaustive Extraction)

Sorbents
Silica-based stationary phase
•Similar to LC phase - C18 most common
•Limited pH stability
•‘Finicky’ to handle
Polymeric
•Stable from pH 1-14
•Not ‘finicky’
 Silica-based SPE cartridges

Procedure:
1. Condition cartridge
C18 tails
2. Load sample
3. Wash co-extractables
4. Elute analytes of interest
Si

Tails ‘solvate’ during step 1

(conditioning), will collapse if
the cartridge goes dry.
Extraction is ruined
 Polymeric SPE cartridges

Procedure:
1. Condition cartridge
2. Load sample
3. Wash co-extractables
4. Elute analytes of interest

F F FF FF F O
F P O
F
F F F F F FF F O

No tails to ‘solvate’, and so

extraction can continue even if
cartridge goes dry
 Polymeric SPE cartridges

+
NH N

+
NH2 NH

F F FF FF F O
F O F P O
F FF FF F F
F P O F F F F F FF F O
F
F F F F F FF F O

Because of the wide pH stability are able to use pH to control

extraction. Very selective and effective extraction technique.
Solid Phase Micro Extraction (SPME)
Only equilibrium extraction method described here.
Often used to observed volatile materials in a
laboratory setting.

N2 in
Sorbent

Sample
Solid Phase Micro Extraction (SPME)

N2 in
Sorbent

Sample
Solid Phase Micro Extraction (SPME)

SPME holder

SPME fibre
Sample
Solid Phase Micro Extraction (SPME)

SPME fiber

Sample