Chem 232 l-l extraction (Ex1)

Chem 232 l-l extraction (Ex1) - October 1st 2008 Separation...

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October 1 st , 2008 Separation of a Mixture of Organic Compounds by Liquid-liquid Extraction Object: The intention of this lab is to achieve either the separation of, benzoic acid from phenanthrene (solution B), or p -bromoaniline from phenanthrene by liquid-liquid extraction, determine the melting ranges of m -toluic acid, p -bromoaniline, and crude and recrystallized phenanthrene, and contrast the purity of recrystallized phenanthrene using both melting ranges and thin layer chromatography. Chemical Equations: Figure 1: Separation and isolation of m -toluic acid from phenanthrene using sodium hydroxide. Figure 2: Separation and isolation of p -bromoaniline from phenanthrene using sodium hydroxide. Procedure Reference: Marrs, P. Chemistry 232 Lab Manual, 2008, 25-30, A-1, A-12, A17, & A-21.
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Experimental Data and Observations: Table 1: Isolated yields. Solution used Mass of phenanthrene Mass of m -toluic acid Mass of p -bromoaniline B 1.70g 1.1g N/A (solution A) Table 2: Recrystallization of phenanthrene. Mass of crude phenanthrene used 0.93g Mass of recrystallized phenanthrene isolated 0.69g Note: Some sample lost from vials after weights taken because of another students misplaced hand knocking over my vials while looking for their vials. Table 3: Melting points of isolated compounds. m -toluic acid p -bromoaniline crude phenanthrene recrystallized phenanthrene 103 o C 60 o C – 61 o C 97 o C 98 o C Observations: The melting range is known as the temperature at which liquid was first observed and the temperature at which the last of the solid melts. For the value above that do not show a range, they did not melt spontaneously when the temperature reached the indicated value, the solid melted over the entire time that the solid was at the temperature. Both of the phenanthrene compounds are suppose to be the same, so it makes sense that
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This note was uploaded on 10/14/2008 for the course CHEM 232 taught by Professor Briggs during the Spring '08 term at University of Victoria.

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Chem 232 l-l extraction (Ex1) - October 1st 2008 Separation...

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