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Page Title:
Protocol II. Accelerated Solvent Extraction One-Step Cleanup |
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 ERDC TN-DOER-C10
March 2000
2) Freeze-dry following instructions provided by the manufacturer. Sediments are
left on the freeze-dryer for at least 24 hours. The vacuum should reach less than
500 10-3 mb for best results.
Protocol II. Accelerated Solvent Extraction One-Step Cleanup.
I.
MATERIALS AND EQUIPMENT.
Dionex Accelerated Solvent Extraction (ASE) 200.
Zymark TurboVap II (Automatic sample evaporator).
MiniVap Evaporator/Concentrator (Supelco # 22971).
33-mL cells for ASE 200.
60-mL collecting vial with Teflon septa.
130 C oven.
Bottle roller.
Balance.
6-in. by 1/2-in.-dowel.
Dionex cellulose filters (1.91 cm).
Funnel.
Freeze-dried environmental sample (2.5 g preweighed).
4-mL amber vial with Teflon-lined polypropylene cap.
Conical inserts and springs for vial (Supelco #60840-639 and #60842A-2).
Safety glasses.
Gloves.
Solvent-resistant gloves.
Dust mask.
II.
REAGENTS.
20-30 Mesh Ottawa Sand Standard.
10 percent dichloromethane (DCM) in hexane.
Hexane (pesticide grade).
Silica gel 60-200 mesh.
Diatomaceous earth.
Concentrated sulfuric acid.
Sulfuric Acid/Silica Gel (SA/SG) (See following preparation instructions).
III.
SA/SG PREPARATION.
Caution! Always wear dust mask, safety glasses, and gloves when preparing SA/SG.
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