Seperation and Extractions Lab Report

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Purpose Extraction is a method used to separate or isolate a particular component of a mixture. This process requires a solvent which allows the desired compound (or compounds) to separate from a solid into a solvent or from a solution into another solvent. In this experiment three compounds were separated; a neutral compound and two weak acids, these compounds are then measured before and after the process in order to determine the efficacy of the separation technique. Reactions 1. Reaction 1:
Transcript
  PurposeExtraction is a method used to separate or isolate a particular component of a mixture. Thisprocess requires a solvent which allows the desired compound (or compounds) to separate from a solidinto a solvent or from a solution into another solvent. In this experiment three compounds wereseparated; a neutral compound and two weak acids, these compounds are then measured before andafter the process in order to determine the efficacy of the separation technique.Reactions1.   Reaction 1: the reaction of p-toluic acid with sodium bicarbonate2.   Reaction 2: the reaction of sodium bicarbonate with acid3.   Reaction 3: the reaction of the major organic product from reaction 1 with hydrochloric acid4.   Reaction 4: the reaction of p-t-butylphenol with sodium hydroxide5.   Reaction 5: the reaction of the major organic product of reaction 4 with hydrochloric acid  C alculations1.   The percent composition of the unknown mixture:2.   The percent recovery of the mixture:ResultsRecovered Mass Percent C ompositionp-Toluic Acid 0.7 58.3p-t-Butylphenol 0.5 41.7AcetanilideDiscussionThe extraction of p-toluic acid was a result of two chemical reactions. To begin the procedure,25 mL of t-butyl methyl ether was placed into a 100mL beaker. Approximately 1.5 grams of theextraction mixture was added and allowed to dissolve; the resulting mixture was then poured into a 125mL separatory funnel (Reaction 1). Next, 10 mL of 0.5M aqueous NaH CO 3 is added to the ether solutionand mixed and shaken until the mixture is gas-free (Reaction 2). The newly formed solution was allowedto separate into two layers: an ether layer and an aqueous layer; the aqueous layer was drained, leavingonly the ether layer remaining within the funnel. This process was repeated twice, and two moreportions of 10 mL NaH CO 3 were added, mixed, and shaken in order to remove any remaining p-toluicacid within the ether layer. The addition of 3M H C l to the NaH CO 3 solution caused a reaction which ledto foaming, ultimately resulting in the precipitation of p-toluic acid (Reaction 3). 3M H C l was thencontinuously added until no more solid is produced and the solution tests acidic (blue litmus paper turnsred). The mass of filter paper was recorded and then used to separate the crystals from the solutionusing vacuum filtration with a Buchnel funnel. The crystals on the paper were placed on a watch glassand allowed to air dry.The remaining ether solution in the separatory funnel is then mixed and allowed to react with10 mL of 0.5M Na O H (Reaction 4). Following this reaction, two layers are formed; drain the Na O H layerfrom the separatory funnel into the 100 mL beaker containing the first Na O H extract. Repeat theextraction of the ether layer by adding a second portion of 10 mL Na O H, and then drain the Na O H layerfrom the funnel into the 100 mL beaker containing the first Na O H extract. After repeating this processwith a third 10 mL Na O H portion, the Na O H solution was then heated to about 60° C on a hot plate in afume hood. 3M H C l was added to the Na O H solution until it became acidic. Next, the mass of the filterpaper was measured, recorded and then used to separate the p-t-butylphenol crystals from the solutionby vacuum filtration with the Buchner funnel. The paper along with the crystals were placed on a watchglass and allowed to air dry.  The ether-acetanilide solution was supposed to be transferred into a clean 125 mL Erlenmeyerflask and then mixed with approximately 1 gram of anhydrous Na2S O 4. In the experiment, Na O H wasadded to the mixture instead of Na2S O 4 producing no visible reaction. As a result, acetanilide wasunable to be isolated ultimately ruining the experiment.There are a few measures that should have been implemented to complete the extractionprocess. During separation, the Na O H layer within the separatory funnel was not extracted carefullyand precisely, leaving a considerable amount within the funnel. Most importantly, human negligenceaccounted for most of the shortcomings during the experiment. The inability to properly followdirections resulted in the incompletion of the extraction process. C onclusionThe extraction process was ultimately a failure. Human error was the predominant factor whichled to the incompletion of the extraction process. C onsequently, the desired result was not achievedand the experiment was deemed a failure. Since the experiment was a failure, the analysis of anysubstitutes was impossible.
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