During the extraction process, the sand bath was set to 20℃. The 1.00 gram of ground nutmeg was transferred to the round-bottom flask (RBF) using the plastic funnel. Three milliliter of tert-butyl methyl ether and two or three boiling chips were added into the flask. The black plastic connector was used just like the distillation column with air condenser set-up. The flask was clamped to the ring stand using 3-pronged clamp. The flask was lowered into a slightly depression in the sand without touching directly to the sand. The mixture was then boiled gently at the boiling point for 10 minutes, removed from the heating, and settled for a minutes. The solids were then left behind while the liquid was transferred into the pressure filtration assembly
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The amount of a milliliter of acetone per 50 mg crude material was added to the 25 mL Erlenmeyer flask. The flask was warmed on the sand bath to dissolve the acid (note: acetone has low BP). The solution was cooled to room temperature for about 5 minutes. If no crystals were formed, scratch the inside surface of flask with glass stirring rod to induce crystallization (note: if still not formed, continue anyway). The solution was cooled in an ice-water bath. The scratching step was repeated when no crystals were formed. The solution was cooled in the ice-water bath for another 15 minutes. Crystals were collected by vacuum filtration on a small Hirsch funnel. The crystals were rinsed. The funnel was lifted slightly to break the vacuum. The crystals were covered with about 1 mL ice-cold acetone. The vacuum was reapplied immediately after. The crystals were air-dried for a few minutes and transferred onto a tared piece of 9 centimeter filtered paper. A melting point of the crystals was obtained using a small sample after the crystals were dried to a constant …show more content…
The available solvents were ethyl acetate and hexanes. Two solvent composition were mixed and created to run the TLC analysis. The solvent of the ratio of 95% ethyl acetate and 5% hexanes and the solvent of the ratio of 95% hexanes and 5% ethyl acetate were created. The TLC analysis was tested to determine which one works the best. The first used composition was recorded. The corresponding TLC plate with circled spots was taped on the notebook. Two solvent systems were kept applying till a decent separation showed between the starting material and the product. To clean up, all wastes were disposed in the Organic Liquid Waste container in the hood. The sand bath was turned off, equipments put away, drawer locked, workspace cleaned up, fume hood closed, and the TA’s signature was obtained before leaving the
The amount of a milliliter of acetone per 50 mg crude material was added to the 25 mL Erlenmeyer flask. The flask was warmed on the sand bath to dissolve the acid (note: acetone has low BP). The solution was cooled to room temperature for about 5 minutes. If no crystals were formed, scratch the inside surface of flask with glass stirring rod to induce crystallization (note: if still not formed, continue anyway). The solution was cooled in an ice-water bath. The scratching step was repeated when no crystals were formed. The solution was cooled in the ice-water bath for another 15 minutes. Crystals were collected by vacuum filtration on a small Hirsch funnel. The crystals were rinsed. The funnel was lifted slightly to break the vacuum. The crystals were covered with about 1 mL ice-cold acetone. The vacuum was reapplied immediately after. The crystals were air-dried for a few minutes and transferred onto a tared piece of 9 centimeter filtered paper. A melting point of the crystals was obtained using a small sample after the crystals were dried to a constant …show more content…
The available solvents were ethyl acetate and hexanes. Two solvent composition were mixed and created to run the TLC analysis. The solvent of the ratio of 95% ethyl acetate and 5% hexanes and the solvent of the ratio of 95% hexanes and 5% ethyl acetate were created. The TLC analysis was tested to determine which one works the best. The first used composition was recorded. The corresponding TLC plate with circled spots was taped on the notebook. Two solvent systems were kept applying till a decent separation showed between the starting material and the product. To clean up, all wastes were disposed in the Organic Liquid Waste container in the hood. The sand bath was turned off, equipments put away, drawer locked, workspace cleaned up, fume hood closed, and the TA’s signature was obtained before leaving the