OCHEM Experiment 7.docx - Briana Palencia CHEM 3321-152 Experiment 7 PreLab Recrystallization Purification of Crude Benzoic Acid and Phenanthrene

OCHEM Experiment 7.docx - Briana Palencia CHEM 3321-152...

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Briana Palencia CHEM 3321-152 3/6/2019 Experiment 7 PreLab: Recrystallization, Purification of Crude Benzoic Acid and Phenanthrene Introduction: The purpose of this experiment is to perform recrystallization on benzoic acid and phenanthrene by dissolving benzoic acid in hexanes and phenanthrene in ethanol/water (solvent pair). Benzoic Acid Phenanthrene Physical Data: Name MW MP (°C) BP (°C) Density (g/mL) Solubility Hazards Benzoic Acid 122.12 2 122.35 249.2 1.27 Soluble in alcohol, ether, and benzene. Slightly soluble in water. Hazardous in case of skin contact (irritant), of eye contact (irritant), of ingestion. Phenanthrene 178.22 9 99.24 340 1.18 Soluble in ethanol, diethyl ether, acetone, benzene, and carbon disulfide. Slightly hazardous in case of skin contact (irritant), of eye contact (irritant). Hazardous in case of ingestion. Chloroform-D 120.38 4 -64 60.9 1.50 Miscible with alcohol, benzene, ether, petroleum Hazardous in case of skin contact
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ether, carbon tetrachloride, carbon disulfide, oils. Soluble in water. (irritant), of eye contact (irritant), of ingestion, of inhalation. Hexanes 86.175 -95.27 68.72 0.661 Soluble in ethanol, ethyl ether and chloroform. Insoluble in water, Hazardous in case of skin contact (permeator), of ingestion, of inhalation. Flammable. Ethanol 46.068 -114.14 78.29 0.789 Miscible with water, ethyl ether, acetone, chloroform. Soluble in benzene Hazardous in case of eye contact (irritant), of inhalation (irritant). May cause drowsiness or dizziness and damage to organs. Flammable. Norite 12.011 3500 N/A 2.70 Insoluble in water. Slightly hazardous in case of skin contact (irritant), of eye contact (irritant), of ingestion, of inhalation. Water 18.015 0 100 1.00 N/A None Procedure: 1. Clean 2 NMR tubes and dry. 2. Obtain 0.10 g of benzoic acid and put it in a small Erlenmeyer Flask. 3. Add 3 mL of hexanes and swirl it. 4. Heat the mixture on the hot plate up to the boiling point (add small portions, about 1 mL, of hexanes until all the soluble material has dissolved) <- use glass rod to crush large chunks of product, don’t go over 10 mL of hexanes.
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5. ->If the solution is colored, remove the hot solution from the hot plate and add a small amount of Norite (1/4 of scapula tip). Swirl and heat up the mixture for about 5 min/ or when the color disappears. If still has color, add a little more of Norite.
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