Extraction:
• Use an aliquot of 150 mL of the water sample.
• Prepare a SPE column with appropriate amount of adsorbent or take a
commercially available SPE cartridge.
• Condition the column according to the instructions given by the SPE
supplier.
• Connect the column to a vacuum pump and hold the column upside down
into the water sample. The flow rate should not exceed 3 mL/min.
• Pump the whole sample volume through the cartridge or column.
• Thereafter, dry the cartridge or column by leaving it connected to the
vacuum pump and allow to pump air for approx. 5 min.
• Elute 5 mL of DCM through the column and collect the extract.
• If applicable add a surrogate standard.
• Prepare a Pasteur pipette by half-filling with Na 2 SO 4 (use glass wool as
stopper at top and bottom)
• After concentration to approx. 1 mL dry the extract over the Na 2 SO 4 filled
pipette and collect the dried extract.
Measurements:
Measure the extract by GC/MS or LC/MS
Standard Operation Procedure SOP 8—Fractionation of Environmental
Solid Matter Extracts (Soils, Sediments . . .)
• Prepare a 2 g silica column. Use only high-quality silica gel. Activate the
silica gel column in the oven at 200
C overnight.
• For conditioning add approx. 5 mL of n-pentane on the top of the column
and let the solvent elute through the bottom of the column. Leave the
column wet.
• Transfer the raw extract (reduced to a volume of approx. 0.5 mL) onto the
top of the column. Let the sample penetrate completely the upper silica
layers.
• Wash the empty extract vial with 0.5 mL of n-pentane and add the washing
solvent also onto the top of the column.
• Add 5 mL n-pentane on the top of the column and collect the percolating
solvent at the bottom as the first fraction.
• Repeat the elution with 8.5 mL of n-pentane/DCM (95:5 v:v) to collect the
second fraction.
• Repeat the elution with 5 mL of n-pentane/DCM (90:10 v:v) to collect the
third fraction.
(continued)
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7 Principal Analytical Procedures in Organic Geochemistry
• Use an aliquot of 150 mL of the water sample.
• Prepare a SPE column with appropriate amount of adsorbent or take a
commercially available SPE cartridge.
• Condition the column according to the instructions given by the SPE
supplier.
• Connect the column to a vacuum pump and hold the column upside down
into the water sample. The flow rate should not exceed 3 mL/min.
• Pump the whole sample volume through the cartridge or column.
• Thereafter, dry the cartridge or column by leaving it connected to the
vacuum pump and allow to pump air for approx. 5 min.
• Elute 5 mL of DCM through the column and collect the extract.
• If applicable add a surrogate standard.
• Prepare a Pasteur pipette by half-filling with Na 2 SO 4 (use glass wool as
stopper at top and bottom)
• After concentration to approx. 1 mL dry the extract over the Na 2 SO 4 filled
pipette and collect the dried extract.
Measurements:
Measure the extract by GC/MS or LC/MS
Standard Operation Procedure SOP 8—Fractionation of Environmental
Solid Matter Extracts (Soils, Sediments . . .)
• Prepare a 2 g silica column. Use only high-quality silica gel. Activate the
silica gel column in the oven at 200
C overnight.
• For conditioning add approx. 5 mL of n-pentane on the top of the column
and let the solvent elute through the bottom of the column. Leave the
column wet.
• Transfer the raw extract (reduced to a volume of approx. 0.5 mL) onto the
top of the column. Let the sample penetrate completely the upper silica
layers.
• Wash the empty extract vial with 0.5 mL of n-pentane and add the washing
solvent also onto the top of the column.
• Add 5 mL n-pentane on the top of the column and collect the percolating
solvent at the bottom as the first fraction.
• Repeat the elution with 8.5 mL of n-pentane/DCM (95:5 v:v) to collect the
second fraction.
• Repeat the elution with 5 mL of n-pentane/DCM (90:10 v:v) to collect the
third fraction.
(continued)
144
7 Principal Analytical Procedures in Organic Geochemistry