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Unformatted text preview: Holly Corbitt 11-16-09 Partner: Shu Chromatography Pu rpose: To learn a common technique to separate and purify compounds of a mixture using column chromatography. Implementing another common chromatography technique to separate and identify components of a mixture using thin layer chromatography. References: Pavia et al. Organic lab techniques 4 th edition. Thompson, Brooks/Cole. 2007 pp. 37 46. Instructor handout. http://msds.chem.ox.ac.uk.html physical properties: Substance Meltin g point Density MW Water Dichlorometha ne Hexane fluorenol 155 C 182.22 g/mol In Sol sol fluorenone 83.5C 1.0728 g/cm 3 180.192 g/mol In Sol sol fluoren e 117 C 1.202 g/mL 166.223 g/mol In Sol sol Safety: Fluorene: Skin, eye and respiratory ir ritant. Shows evidence in laboratory animals of mutagenic properties. ATSDR minimal risk level ORL 0.4 mg/kg/day. Toxicological properties not fully investigated. Fluorenone : Hazardous in case of skin contact (irritant), of eye contact (irritant), of ingestion. Combustible. Fluorenol : Combustible, not a hazard Dichloromethane : Harmful if swallowed or inhaled. May be harmful by skin contact. Eye and skin ir ritant. Readily absorbed through the skin. Asphyxiant. Causes CNS depression. Possibly carcinogenic in humans. Possible mutagen. Experimental reproductive effects. Hexane : May cause impaired fertility. Harmful by inhalation. I r ritant. May cause CNS depression. Prolonged exposure may cause serious health damage. Stable. Incompatible with oxidizing agents, chlorine, fluorine, magnesium perchlorate. Highly flammable. Readily forms explosive mixtures with air. Note low flash point. Procedure : Part A: Using a lead pencil draw a line 1 cm from the bottom of the TLC plate and mark with five tick marks to indicate where each solution will be placed. Prepare the solvent, methylene chloride and hexane, by putting enough to cover the bottom of a wide mouth beaker and cover with tin foil, to prevent evaporation. Put a drop of each solution; 1- unknown C, 2-fluorenol, 3-fluorene, 4-fluornone, 5-reference mixture; on the corresponding mark using a capillary tube, wait for them to dry, and then place bottom first into beaker, cover. Wait until solvent has been drawn up by the plate, about 2 cm from the top, and mark with pencil. Set on a piece of towel and wait for the plate to dry. Using a UV light wand with pencil....
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