Aims of Experiment
- To isolate trimyristin from a natural product, named nutmeg, using solvent extraction.
- To purify the isolated trimyristin by recrystallization.
- To get infrared spectrum of the isolated trimyristin.
Introduction
Many natural products such as medicine and cosmetic which are extracted from animals and plants are around us. Like this, Trimyristin, which is composed of triglycerides, is that it can be isolated from nutmeg seed. It is widely used as hair conditioner or oil. One of the important method to extract pure trimyristin from nutmeg is reflux condenser. The reflux condenser is used in case that we want to prevent organic compound with volatile substance or solvent from being evaporated while heating and cooling occur
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After setting the apparatus, put 15g of ground nutmeg seed and 40ml of acetone into the 100ml round bottom flask. Then, put the flask into the heating mantle and heated it up for 15 minutes while shaking smoothly. During this process, made hot water to preheat the stemless funnel and conical flask to about 80 ℃ and also made 32-fold filter paper. After 15 minutes, keeping our solution in 100ml round bottom flask hot with heating mantle, poured our solution into filter paper in the preheated stemless funnel and conical flask smoothly. Added 15ml of acetone to wash the residue and poured all liquid of our solution. Then, placed extracted liquid into an ice bath to get crystallized and after putting some acetone on the flask, isolated the solid material by suction filtration using Buchner …show more content…
Then filtered the solution quickly with the stemless funnel, 32-fold filter paper and conical flask. To get more colorless liquid, repeated this process 3 times. Then, placed the conical flask in an ice bath and waited until crystallization finished. Isolated the purified product by suction filtration. Finally, put half spoon of recrystallized product and Nujol powder in an agate mortar and grinded finely. Then, made the mull and transferred the mull to the bottom salt plate of a demountable cell. Then run the spectrum.
Precautions
Acetone, which used to mix with ground nutmeg seed and wash the residue, is not very toxic but highly flammable and also has easily evaporable property. From this reason, we have to pay special attention to flame around us when doing experiment.
Paraffin, which composes paraffin oil, is also flammable so that it can catch fire easily.
When adding ground nutmeg seed, acetone and heating it with heating mantle, it is important to gently swirl the solution to avoid bumping. It can be more secure to add anti-bumping
Experiment 55 consists of devising a separation and purification scheme for a three component mixture. The overall objective is to isolate in pure form two of the three compounds. This was done using extraction, solubility, crystallization and vacuum filtration. The experiment was carried out two times, both of which were successful.
Add the powder into a 100mL volumetric flask by using the folded side of the weighing paper. Gently slide the solid into the flask. Use distilled water to rinse the weighing paper into the flask. Fill the flask to the mark with distilled water. Then cap the flask with parafilm and mix thoroughly. This solution is now known as Master Solution. After rinsing the pipet three times with a small amount of the master solution, pipet exactly 10.00 mL of the master solution into a clean dry 250 mL Erlenmeyer flask. One should then repeat step 6 so that one should have three flasks with 10mL of the master solution in each. Then rinse the pipet three times with distilled water. Following that, rinse the pipet three times with a small amount of hydrochloric acid. Pipet exactly 10.00 mL of hydrochloric acid into each of the three flasks and swirl the flasks to make sure the solutions are mixed all the way. The solution should now be a yellowish precipitate. For part three, one should first rinse the buret three times with distilled water, then rinse the buret three times with a small amound of sodium hydroxide. Fill the buret with about 40mL of the sodium hydroxide solution and put the buret in a secure buret
*Peanut oil has a higher smoke point and has less of a chance of burning during the experiment.
The two peaks next to each other, 2360.23 cm-1 and 2341.78 cm-1, most likely indicated a nitrile or alkyl stretch. These peaks disappeared in the spectrum for the crystallized 3-nitrochalcone, though. The peaks were most likely as the result of an incomplete reaction or a reaction that did not go to completion. The product probably did not completely tautomerize, showing an alkyl or nitrile group. The crude product was also not completely dried, as indicated from the presence of an -OH group at the 3383.38 cm-1 peak. Figure 2 depicts the infrared spectrum of the crystallized product. The two peaks, signifying the nitrile or alkyl stretch, were still on the spectrum, but smaller. However, a peak at 3380.36 cm-1 indicates that an OH stretch is still present in the crystallized product. This verifies that the product was not pure; that –OH group was likely from methanol, the solvent used to purify the crude product. In order to remove the methanol/OH group, the crystallized product was left to dry in an oven for several minutes to spur dehydration. After that, another IR spectrum was taken for the dried product (Figure 3). In this spectrum, there was no alcohol peak, which indicates that the product became pure; the compound lost the hydroxyl group and no methanol was found in the pure product. As a result, Figure 3 is the desired
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