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Lab Practical Procedure

1. The document describes the procedure for extracting and purifying an unknown organic solid, including steps for extraction with an organic solvent, water washing, drying, filtration, rotary evaporation, recrystallization, and analytical techniques. 2. The recrystallization process involves dissolving the isolated solid in ethanol and cooling to form crystals, which are then filtered, dried, and weighed. 3. Analytical techniques to identify the unknown substance include obtaining the infrared spectrum, measuring the melting point range, and comparing the results to known compounds.

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Alyssa Ference
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39 views

Lab Practical Procedure

1. The document describes the procedure for extracting and purifying an unknown organic solid, including steps for extraction with an organic solvent, water washing, drying, filtration, rotary evaporation, recrystallization, and analytical techniques. 2. The recrystallization process involves dissolving the isolated solid in ethanol and cooling to form crystals, which are then filtered, dried, and weighed. 3. Analytical techniques to identify the unknown substance include obtaining the infrared spectrum, measuring the melting point range, and comparing the results to known compounds.

Uploaded by

Alyssa Ference
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd
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Alyssa Ference

Dr. Moerdyk

SCH 211 01

16 October 2018

Lab Practical Procedure

Extraction

1. Collect the unknown solid and measure the mass. Should be approximately 2 g. Then, set up

the separatory funnel apparatus.

2. Add 5 mL of methyl- tert- butyl ether to the separatory funnel to test it for leaks and then

transfer the unknown organic solid into the funnel using a powder funnel.

3. Add 20 more mL of methyl-tert-butyl ether and swirl until the solid dissolved.

4. Use two 15 mL portions of water to extract the ether. Be sure to periodically vent the funnel

and invert it to allow the two layers to form. The bottom layer should be the blue water-soluble

dye and water while the top layer should be the unknown solid and methyl-tert-butyl ether.

5. Use 15 mL of saturated NaCl to remove excess water in the remaining organic layer. Then

decant the organic layer in a new beaker and discard the remaining NaCl.

6. Drain the organic layer into a clean, dry 50 mL Erlenmeyer flask through the top of the funnel.

7. Add approximately 0.5 g of Na2SO4 to the flask as a drying agent.

8. Once there are free flowing crystals in the flask, retrieve and weigh an empty and dry 100-mL

round-bottomed flask.

9. Filter the solution in the Erlenmeyer flask to the 100-mL round-bottomed flask through the

fluted paper.
10. Evaporate the solution in the round-bottomed flask by rotary evaporating it until it is dried,

then reweigh the round-bottomed flask with the isolated solution in it.

Recrystallization

1. After weighing the unknown substance, transfer it from the 100-mL round-bottomed flask to a

large diameter test tube. Rinse with the recrystallization solvent, ethanol, by adding 5 grams of

ethanol per gram of unknown substance.

2. Once the unknown substance is added to the large diameter test tube, place it into a warm

water bath with a thermometer and a boiling stick.

3. Use a Pasteur pipette to add water from a graduated cylinder in periods of drops until a cloudy

point begins to show. If a cloudy point is reached, add ethanol to produce a clear solution.

4. Allow the solution to cool until it reaches room temperature. Then, transfer the test tube to an

ice water bath.

5. Once the crystals form, suction filter and wash them with a few mL of cold ethanol. Pull air

through the crystals for around 3 minutes to dry the crystals.

6. Transfer the crystals to a clean, dry beaker for air-drying. Then, weigh the product, determine

the melting point range, and obtain the IR spectrum.

Analytical techniques

1. Weigh the unknown substance crystals before performing any of the techniques.

2. Perform the IR spectra using a small amount of the crystals.

3. Place a small amount of the crystals in a thin test tube to analyze the melting point range as it

is heated.

4. Determine the unknown substance by using the results from the IR and the melting point

range.

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