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Orgo Lab Report Extraction Nov 17 2011.docx

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CHEM 203
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Separation of an AcidNeutral Mixture by LiquidLiquid Extraction thOct 28Nov 4 2011 PURPOSE Liquidliquid extraction was performed as a method to separate compounds in an impure mixture in our experiment vanillin and cholesterol This technique was dependent upon the solubility differences of each of the two compounds in a mixture of solvents PROCEDURES Refer to pp 4144 of the CHEM 23202420 of the Laboratory Manual Fall 2011 Edition for the procedures of this experimentAn extra three dropper full of dichloromethane DCMin addition to the small amountwas added to rinse the sample mixture into the sep funnel No distilled water was used during this rinsingWhile repeating the extraction with 10NaOH to remove vanillin from the organic layer the top layer NaOH extract was mistaken as the organic layer by error and was kept in the sep funnel while the bottom layer containing most of the cholesterol was placed in the NaOH extract flaskDue to having added too much drying agent MgSO4 anhydrousa gravity filtration using a longstem funnel and cheesecloth was used to facilitate passage of the vanillin and cholesterol filtrateMeasurements of the mass of beakers used for crude vanillin and crude cholesterol were omitted by mistake Products in their solvent were left in their respective beaker covered with Kimwipes to evaporate at room temperature in lieu of evaporation by use of a hot water bath During the second week of the experiment cholesterol sample from lab instructor was supplied and added to the crude cholesterol product obtained from the previous week to continue the experiment with recrystallization of the crude cholesterolIn lieu of hot gravity filtration decanting was used to separate insoluble impurities in solvent In lieu of a solventsaturated filter paper parafilm was used to tightly seal and facilitate saturation of the mobile phase solvent mixture in TLC beaker OBSERVATIONSDichloromethane mixed with Vanillincholesterol sample appeared colorlessWhen NaOH was added to the above mixture the solution became light yellowish in color with oil droplets sitting on the topIn the sep funnel the vanillincholesterol mixture in NaOH solution and CH2Cl2 formed two layers the top layer being yellow in color and the bottom layer appeared colorlessSmall amounts of gas released between mixing Cheryl Lee100191898
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