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Sample extraction
Procedures prior to analysis
Air sample
Cold-extraction
Soxhlet extraction
PR Extraction
Oscillating extraction
Soil sample
Solvent immersing extraction
Oscillation extraction
Ultrasonic extraction
Immersing the homogenized sample in extraction solvent
Oscillating the sample
Sucking filtration of samples Sucking filtration
Concentrate the eluent.
PR Extraction
Crop or animal tissue
Rinse
Oscillating
Blending or homogenizing
Soxhlet extraction
Digestion
Extraction solvent
PR Extraction
1Inertness.
Digestion method No chemical reaction with the solvent, no effect to the
Acid digestion equipment.
Alkali digestion
Enzymatic digestion 2Purity.
Testing method
300500mL of solvent is concentrated with K-D
Microwave assisted digestion
Apparatus to 35mL.
the homogenized fish sample is treated by No interferences peak in GC-ECD with 2 microliter
20mL mixture of 4:1 glacial acetic acid and injection.
perchloric acid, seal the sample and put it in
microwave oven.
Homework title
Supercritical FluidSF
Supercritical Fluid Extraction
Gas SF Liquid
(cm2/s)
Ideal extraction solvent, SF Ideal extraction solvent, SF
Solvent Strength of SF decreases with the decreasing 3. Lower viscosity than liquid solvent
pressure. When the pressure decreases to atmospheric pressure, It could penetrate into porous solid materials more effectively
the SF loses the dissolving power and the extracted compounds than liquid solvents and, consequently, it may render much faster
settle out. mass transfer resulting in faster extractions.
scCO2
5. To improve the solubility, by adding some cosolvents, or Easy to obtain the critical condition
called entrainers, modifiers sc CO2Tc31.lPc7.38MPa
Low price, low toxicitynon-ignitibilitylow boiling point,
released to environment after extraction at normal pressure
Although scCO2 has bipolar and good dissolving capacity,
Only fit to the non polar or low polar compound.
cosolvents should be added to compete active sites with
analytes when SF is used to extract polar compounds. The Advantage of SFE:
addition of cosolvents could increase the dissolving capacity Volume of organic solvent was reduced
and enhance the extraction efficiency. In addition, Time of extraction was reduced.
cosolvents could improve the selectivity of the extraction. Disadvantage, expensive equipment
Methanolethanolisopropanol<10
Polar comparison
CAR - TPRPDMS - DVB PA PDMS PDMS
Solid Phase Micro Extraction Extraction efficiency with T
50
SPME mode
a Dir-SPME
b HS-SPME
c membrane-protected SPME
Upon shaking and centrifugation, an aliquot of the organic phase Vortex 1min and centrifuge
is subjected to further clean up using SPE. Unlike traditional
methods using SPE tubes, in dispersive SPE, clean up is 1 mL supernatant + 50mgPSA + 150 mg anhydrous MgSO4
facilitated by mixing bulk amounts of SPE (e.g., Supelclean PSA,
Vortex 1min and centrifuge
ENVI-Carb, and/or Discovery DSC-18) with the extract.
500L extract into autosampler
After sample clean up, the mixture is centrifuged and the resulting vial for LC / GC analysis
supernatant can either be analyzed directly or can be subjected to
minor further treatment before analysis.
2003
GC-NPD
DSPE
Homogenized sample was mixed with 40mL
ethyl acetate, 15g Na2SO4, 5g NaCl, 1g florisil, The proportion of florisil
0.05-0.1g activated carbon Different proportion florisil ( 0%2.5%5%10% 20% )
Fortified cabbage sample
was added into10g sample .
CH3CN was alternative Result shows that good recovery was obtained at 10% of florisil
addition .
DSPE
Without
0.5 g portion sample
r-DSPE r-DSPE
r-DSPE (PSA) (MWCNTs)
0.5 g of C18-bonded silica
Multi-Residue Analysis
standard
Matrix effect-fenamiphos
evaporated under N2
DSPE Clean-up MgSO4+PSA+C18
GC-MS
neutral surfactants
P113
KD evaporators
Rotating film (vacuum) evaporators
Gas stream concentrator
-gradually lower the distillation flask into the water bath until
evaporation starts; keep the boiling process well under control at
all times (if this is not the case, lift the flask from the water bath
and lower the temperature of the water);
-do not fill the distillation flask for more than 1/2 of its volume;
- lift the distillation flask from the water bath as soon as the
- firmly fix the distillation flask to the evaporator by means of a volume of the remaining liquid is approx.2-3 ml; do not
clamp; evaporate to complete dryness;
- slowly start rotation so that an even distribution of the liquid - slowly release the vacuum;
over the inner wall of the flask is obtained; do not let the flask
turn at a higher speed than necessary;
When only small amounts of co-extractives are present in the Solvent which has less volume and higher volatility.
extract to be concentrated, and when the pesticides to be Pesticide which has lower vapor pressure.
determined are volatile, losses during the evaporation
procedure can occur. This can be circumvented by adding an
inert holder, such as n-hexadecane. A useful quantity is 2
ml of a 0.2% solution in n-hexane in a 500 ml evaporation
flask.
Henrys constant =f (vapor pressure/ solubility) Vapor dynamic headspace enrichment device
Fit to VOC
3Concentration method