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Joint International Conference on Long-term Experiments ...

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Column Chromatography<br />

Loosely place glass wool plug in bottom of chromatographic tube and add ca 15 g<br />

anhydrous sodium sulfate. Add 4 g cupric carb<strong>on</strong>ate-diatomaceous earth (1 + 2); lightly<br />

pack column by holding in upright positi<strong>on</strong> and by allowing it to drop gently <strong>on</strong> its tip <strong>on</strong>to<br />

book or writing pad. Add 20 g sodium sulfate to top of column.<br />

Sequentially pass methylene chloride extracts through column, beginning with 50 mL<br />

porti<strong>on</strong>. Collect that eluate and each successive eluate in 250 mL Philips beaker. Add 25 mL<br />

porti<strong>on</strong> to column when first porti<strong>on</strong> has drained to below top layer of sodium sulfate. Rinse<br />

column with 10 mL methylene chloride.<br />

Add 4-5 SiC boiling chips to Philips beaker and evaporate solvent nearly to dryness <strong>on</strong><br />

steam bath under gentle stream of nitrogen. Cool to room temperature and quantitatively<br />

transfer with small porti<strong>on</strong>s of methylene chloride to 5 mL vial. Evaporate solvent to<br />

dryness under gentle stream of nitrogen. Save sample residue for TLC.<br />

This Layer Chromatography<br />

Add 100 μL benzene (screen < 10 ppb) or 200 μL benzene (screen1<br />

h before using.<br />

Spot plate as previously described and develop using benzene-methanol (95 + 5).<br />

Solvent fr<strong>on</strong>t travels 13-15 cm in 45 min.<br />

563

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