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Purification Of 4-Dibromobenzene

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Experiment Title: A Separation and Purification Scheme. Kunal Patel T.A: Justin Maxwell 2460-008 November 8, 2016 Introduction: This experiments main purpose was to separate and purify the components of the unknown substance given. The unknown had been allotted in the lab according to the initials of the last name. The three unknown components were 50% o-toluic acid, 40% fluorene and 1,4-dibromobenzene. This lab was essential because each student had to create the lab protocol for the lab. This helped us to know more about the techniques we used in previous labs. The given components of the mixture were separated and purified by an acid-base extractions and crystallizations. From the three components at least two of them was separated and purified and helped to …show more content…

The solid recovered from the aqueous layer was obtained as o-toluic acid and the solid from the organic layer was obtained as fluorene. The aqueous layer contained the sodium hydroxide salt of o-toluic acid after the addition of NaOH due to its acidic nature. When 1M HCl added, o-toluic acid was precipitated out of the solution as it is insoluble in it. The solid could be obtained from vacuum filtration. The two components of the organic layer were separated according to the solubility properties. Fluorene was precipitated when the sodium sulfate solution was added to the organic layer. As a result, the solubility of fluorene was decreased further when it was placed in an ice-water bath. Fluorene could also be obtained using vacuum filtration and 1,4-dibromobenzene remained in the fluorene solution due to its higher solubility. As it was 10% of the whole mixture, it is considered to be 1,4-ibromobenzene was the minor product and thus could be rejected. The melting point range was used to identify the unknown solids from the mixture. 91.01% yield for o-toluic acid and 72% yield for fluorene was calculated

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The percent recovery of the acid was 42%, but there was originally 40% of o-toluic acid in the mixture. The extra 2% could have been the impurity, 1, 4-dibromobenzene, which was isolated in the next part of the experiment. There is also another possible reason on why more acid was recovered. The acid wasn’t dried completely before it was weighed; the clumpy solids of the acid prove that it was still wet and thus, the extra liquid added to its mass. This could have been prevented by allowing the acid to dry longer or by drying it in an oven.

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