Standard Operation Procedure SOP 1—Solid Matter Soxhlet 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 Soxhlet device that will have contact with the
sample.
Extraction:
• If applicable add an internal standard to the sample.
• Fill an appropriate amount of solid sample material (depending on the TOC
value) into the extraction tube.
• Fill an appropriate amount of extractant (e.g. DCM, acetone . . . .) into the
Soxhlet device.
• Start the first extraction cycle by heating the solvent.
• After 48 h of extraction the solvent can be changed to a less polar one
(e.g. to n-hexane) if a more exhaustive extraction is needed. Start a second
extraction cycle.
• After exhaustive extraction filtrate the raw extract and reduce the extract
volume by rotary evaporation.
• Prepare a Pasteur pipette by half-filling with Na 2 SO 4 (use glass wool as
stopper at top and bottom, see on the right).
• After concentration to approx. 1 mL dry the raw extract 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
7.1 Analyses of Fossil Matter
137
(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 Soxhlet device that will have contact with the
sample.
Extraction:
• If applicable add an internal standard to the sample.
• Fill an appropriate amount of solid sample material (depending on the TOC
value) into the extraction tube.
• Fill an appropriate amount of extractant (e.g. DCM, acetone . . . .) into the
Soxhlet device.
• Start the first extraction cycle by heating the solvent.
• After 48 h of extraction the solvent can be changed to a less polar one
(e.g. to n-hexane) if a more exhaustive extraction is needed. Start a second
extraction cycle.
• After exhaustive extraction filtrate the raw extract and reduce the extract
volume by rotary evaporation.
• Prepare a Pasteur pipette by half-filling with Na 2 SO 4 (use glass wool as
stopper at top and bottom, see on the right).
• After concentration to approx. 1 mL dry the raw extract 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
7.1 Analyses of Fossil Matter
137