Separation by Extraction
Essay by Sicong Liu • October 25, 2017 • Lab Report • 1,161 Words (5 Pages) • 1,432 Views
Chemistry 232 Fall 2017, Spring and Summer 2018
Separation by Extraction
Name: Date: Oct. 1st, 2017
Abstract
The objectives of this lab were to extract crude phenanthrene, benzoic acid and p-chloroaniline from two stock solutions by using liquid-liquid extraction, and to recrystallize the phenanthrene. Then, the purity of these compounds was evaluated by the melting point range, the solubility and the thin layer chromatography (tlc) test.
Equation of Extraction and Regeneration of Components
Procedure Reference
Refer to Peter, M. Chemistry Laboratory Manual 232, pp21-27 (University of Victoria: Victoria, BC) Fall 2017.
Liquid-liquid Extraction
Reagents for Extraction--indicate which stock solution was extracted!
Compound(Reagents) | MW(g/mol) | Used | Mole | Physical and Safety Data |
p-chloroaniline (1.00g/100mL) and phenanthrene (2.00g/mL) (Solution A) ClC6H4NH2 | 127.57 | 100mL | 0.00784 | Bp: 232°C，mp：67-70°C，Acute toxicity (oral, dermal, inhalation) ，Health Hazard，Hazardous to the aquatic environment |
Benzoic acid(1.00g/100mL) and phenanthrene (2.00g/mL) (Solution B) C6H5COOH | 122.12 | 100mL | 0.00819 | Bp: 249°C，mp：121-123°C，corrosion，Health Hazard |
Phenanthrene C14H10 | 178.23 | 1.006g | 0.00561 | Bp: 232°C，mp：67-70°C，Colorless monoclinic crystals with a faint aromatic odor, solution exhibit a blue fluorescene. Harmful if swallowed, very toxic to aquatic |
Dichloromethane CH2Cl2 | 84.93 | 0.5mL | Solvent | Mp: 91, bp:340, density: 1.325g/ml, toxic, irritant, carcinogen |
Hydrochloric acid HCl | 36.46 | 3*30mL | 37% by weight in water, d 1.20/ml, concentration is 12M. highly toxic, corrosive. This is also true of the 6M and 3M solutions used. Dispose as acidic aqueous waste. | |
Sodium hydroxide NaOH | 40.00 | 3*30mL | d 2.13g/ml. corrosive, toxic. This is true of the aqueous solutions used. Dispose in “basic aqueous waste” container | |
Water H2O | 18.02 | Solvent | Mp 0°C, bp 100°C, d 1.00g/ml. | |
Ethanol C2H5OH | 46.07 | Solvent | Bp 78°C, d 0.790g/ml. flammable liquid, irritant. Excess consumption on may lead to social consequences. Dispose as non-halogenated wasted | |
Sodium sulfate NaSO4 | 142.04 | 3.750g | Solvent
| D 1.84g/ml, Highly toxic, corrosive oxidizer. This is true for aqueous solutions. Dispose by neutralizing, and flushing down the sink with running water. |
Hexane
| 86.18 | Solvent | D 0.659g/mL, bp 69°C, mp -95°C. flammable liquid, irritant. Dispose as non-halogenated waste. | |
Toluene C6H5OH | 92.12 | Solvent | D 0.865g/mL, bp 110-111°C, mp -93°C. flammable liquid, toxic | |
Cyclohexane C6H12 | 84.16 | Solvent | D 0.779g/mL, bp 80.7°C, mp 4-7°C. flammable liquid. Dispose as non-halogenated waste. | |
Ethyl acetate | 88.11 | Solvent | D 0.902g/mL, bp 77.1°C, mp -83.6°C. flammable liquid. Dispose as non-halogenated waste. | |
p-anisaldehyde CH306H4CHO | 136.15 | stain | D 1.119g/mL at 25°C (lit.), bp 248°C, mp -1°C. Hazardous in case of ingestion, skin contact and eye irritant | |
Bromocresol green C21H14Br4O5S | 698.01 | stain | Mp 225°C. irritant to eye and skin |
Recrystallization of Phenanthrene
Compound | MW (g/mol) | Used | moles | Physical and Safety Data |
Recrystallized Phenanthrene | 178.23 | 1.006g | 0.00561 | Bp: 232°C，mp：67-70°C，Colorless monoclinic crystals with a faint aromatic odor, solution exhibit a blue fluorescene. Harmful if swallowed, very toxic to aquatic |
Benzoic acid | 122.12 | Bp: 249°C，mp：121-123°C，corrosion，Health Hazard | ||
p-chloroaniline | 127.57 | Bp: 232°C，mp：67-70°C，Acute toxicity (oral, dermal, inhalation) ，Health Hazard，Hazardous to the aquatic environment |
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