Sand Bath Lab Report

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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 …show more content…
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 2 mL of 6 M NaOH, 2 mL of 95% ethanol and a boiling chip were added in order to reflux gently on the sand bath for 45 minutes. If less than 60 mg of trimyristin obtained, the hydrolysis was scaled down by a factor of two. Only half of the amounts of all reactants – trimyristin, NaOH, and ethanol – were used to experiment. The reminder of liquid in RBF were examined in order to replace ethanol if necessary for a continuous boiling. During hydrolysis, the remaining trimyristin were recrystallized a second time. The solution was cooled down to room temperature for 10 minutes. Then, the solution was cooled in an ice bath for 10 minutes. In this second recrystallization, trimyristin was dissolved in the minimum amount of acetone at the boiling point of the solution. The product was collected via the vacuum filtration and dried to a constant weight. The melting points of the first recrystallized and second recrystallized trimyristin were compared. After 45 minutes of hydrolysis, the flask was cooled to the room temperature. The contents were poured into a 50 mL beaker containing 8 mL of water. In the fume hood, 2 mL of concentrated HCl was added dropwise while stirred carefully. At the end, the myristic acid precipitated. If the gelatinous solid is observed, then HCl might not be enough or the solution needed more stirrings. The beaker was cooled in

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