Standard Operation Procedure SOP 2—Solid Matter Extraction by ASE
(Accelerated Solvent Extraction) (Rocks, Sediments, Soils, Coals . . .)
Preconditions:
• Clean all needed glass material by rinsing it with DCM and make sure to
use only glass, metal and PTFE equipment.
• Use only precleaned (distillation) or ultra-pure solvents.
• Rinse the all parts of the ASE that will have contact with the sample.
Extraction:
• Choose an appropriate cell depending on the TOC content.
• If applicable add an internal standard to the sample.
• Fill the sample as well as beads into the precleaned cell. Make sure that the
cell is filled completely.
• Start the automatic extraction cycle. Observe the pressure. In case of
excessive pressure check if the filter is blocked.
• After extraction let the cell cool down, disassemble the cell completely and
clean the filters and metal rings in the ultrasonic bath with organic solvent
for 15 min.
• Concentrate the extract to approx. 1 mL.
• Switch extract solvents from DCM to n-hexane by adding approx. 2 mL of
n-hexane to the raw extract and concentrate the sample by rotary evaporation. Repeat this procedure twice.
• 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 n-hexane phase over a Na 2 SO 4
filled pipette and collect the dried extract
• For desulphurization, add freshly activated copper powder (activation with
HCl) to the sample and leave it in the refrigerator overnight.
Further handling:
Proceed with fractionation of the desulphurized raw extract
Standard Operation Procedure SOP 3—Solid Matter Extraction by
Ultrasonication (Rocks, Sediments, Soils, Coals . . .)
Preconditions:
• Clean all needed glass material by rinsing it with DCM and make sure to
use only glass, metal and PTFE equipment.
• Use only precleaned (distillation) or ultra-pure solvents.
(continued)
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7 Principal Analytical Procedures in Organic Geochemistry
(Accelerated Solvent Extraction) (Rocks, Sediments, Soils, Coals . . .)
Preconditions:
• Clean all needed glass material by rinsing it with DCM and make sure to
use only glass, metal and PTFE equipment.
• Use only precleaned (distillation) or ultra-pure solvents.
• Rinse the all parts of the ASE that will have contact with the sample.
Extraction:
• Choose an appropriate cell depending on the TOC content.
• If applicable add an internal standard to the sample.
• Fill the sample as well as beads into the precleaned cell. Make sure that the
cell is filled completely.
• Start the automatic extraction cycle. Observe the pressure. In case of
excessive pressure check if the filter is blocked.
• After extraction let the cell cool down, disassemble the cell completely and
clean the filters and metal rings in the ultrasonic bath with organic solvent
for 15 min.
• Concentrate the extract to approx. 1 mL.
• Switch extract solvents from DCM to n-hexane by adding approx. 2 mL of
n-hexane to the raw extract and concentrate the sample by rotary evaporation. Repeat this procedure twice.
• 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 n-hexane phase over a Na 2 SO 4
filled pipette and collect the dried extract
• For desulphurization, add freshly activated copper powder (activation with
HCl) to the sample and leave it in the refrigerator overnight.
Further handling:
Proceed with fractionation of the desulphurized raw extract
Standard Operation Procedure SOP 3—Solid Matter Extraction by
Ultrasonication (Rocks, Sediments, Soils, Coals . . .)
Preconditions:
• Clean all needed glass material by rinsing it with DCM and make sure to
use only glass, metal and PTFE equipment.
• Use only precleaned (distillation) or ultra-pure solvents.
(continued)
138
7 Principal Analytical Procedures in Organic Geochemistry