Essay about Investigating The Separation And Purification Technique

Essay about Investigating The Separation And Purification Technique

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The objective of this experiment was to perform extraction. This is a separation and purification technique, based on different solubility of compounds in immiscible solvent mixtures. Extraction is conducted by shaking the solution with the solvent, until two layers are formed. One layer can then be separated from the other. If the separation does not happen in one try, multiple attempts may be needed.
The experiment was conducted in three parts: Part A of the experiment consisted of extracting caffeine from an aqueous solution; Part B consisted of using three different compounds: benzoic acid, succinic acid, and sodium benzoate; and the last part of the experiment consisted of using a solid neutral compound with an acid or base impurity.
For the first part, 0.170 g of caffeine was used. This was dissolved in water and 5 ml of methylene chloride was used to extract it from the aqueous solution. A 125 ml separatory funnel was initially used to shake the solution with the solvent. When two liquid layers were formed, the organic layer at the bottom that had most of the desired product was separated from the other for three consecutive times and emptied into an Erlenmeyer flask from the methylene chloride was evaporated. The end product was 0.060 g of purified caffeine. This was a yield of 35.29 percent.
For the second part, a team of three worked on the extraction of benzoic acid, succinic acid, and sodium benzoate. The testing was conducted to determine how the organic solids were distributed between methylene chloride and water. The process was similar to Step A, and after evaporation was conducted, the end product was 0.045 grams of sodium benzoate. The distribution coefficient was 0.818.
For the last part, a solid n...


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...paratory funnel between 1.0 M NaOH and the solution with the unknown mixture. The extraction started with 0.36 grams of the unknown mixture and yielded as the end product 0.251 grams of the purified neutral compound. This resulted in a percent yield of 69.72%. Some possible sources of loss could have been liquid lost when transferred into the Erlenmeyer flask. Also in the first step, when 0.36 grams of the unknown mixture was placed on the filter paper for measuring, some of the mixture might have stuck to the filter paper when pouring it into the screw-cap centrifuge tube. The melting point of the compound in the end was measured as 81-84* Celsius. This melting point range falls in the melting point range of fluorenone which is 82-85* Celsius. Therefore, it can be said with some degree of certainty that the neutral compound in the impure sample was fluorenone.

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