Experiment 1: Recrystallization – Evaluation Summary
Last Name: Xavier
First Name: Jessica
Date: October 1st 2013
Lab Day/TA/Group: Wednesday(1:35pm)/Group A
Labs reports must be typed and chemical structures must be drawn with ChemDraw. Report must not exceed three pages (including this page). Page limit does not include any attached spectra or references.
** Deductions for hand written report/structures and exceeding page limit **
Report Breakdown Data/Results: _________________ /10
Discussion: _________________ /10
Report Total: _________________ /20
Other Lab Marks Performance: _________________ /6
Prelab Quiz: _________________ /3
TA Comments on Report/Performance
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Given the following solubility test results, which would be the best recrystallization solvent for Compound A? Why?
Ethanol: Cold – soluble; Hot – soluble
Water: Cold – insoluble; Hot – soluble
Benzene: Cold – insoluble; Hot - insoluble
Water would be the best recrystallization solvent for Compound A, because when doing recrystallization, it is important that the compound be very soluble at the boiling point, and hardly soluble at room temperature. If it were insoluble in hot temperatures the compound would not dissolve, where as if it was soluble in cold, crystillization would be a very unlikely process. To note, impurities should on the other hand be very soluble at room temperature and insoluble in hot solvent in order to be filtered out due to the fact they remain dissolved in the solvent where as the rest of the compound crystallizes when cooling.
2. How does recrystallization purify a solid?
-First a saturated solution is made(a compound containing impurities is dissolved in a hot solvent)
-Secondly, the solution is cooled slowly(the slower, the bigger the eventual crystals), allowing solubility of compound to drop(not impurities solubility however), starting the crystillization process. (to note, to start the crystillization of the compound a seed is often required which involves scratching the glassware until a nucleus of glass
The product was then suspended in 2 ml of water with a stir rod in a 50 ml Erlenmeyer flask and heated to boiling. Water was added in one milliliter increments until all the product was dissolved (18 ml added total). The saturated solution was allowed to slowly cool, and gradual white crystal formation was observed. Recrystallized product was collected once more by suction filtration with the Hirsch funnel once crystallization ceased. Collected product dried on a watch glass for a week, weighed 0.14 g (1.2 mmol), and the melting point was 139°-141°
During recrystallization, the solution was to be cooled to room temperature before placing it in an ice bath. Doing this allows enough time for the crystals to be formed because as the temperature decreases, the rate of crystallization slows down. If the solution was placed in the ice bath too quickly, then the cold would have blocked out the impurities and trapped them in the solution. The more impurities present, the lower the melting point so data would have been inaccurate. Also, if the melting point apparatus wasn’t set up correctly, the data would have been imprecise.
Phenacetin’s cold water solubility is 0.076 grams/100 mL of water, whereas its boiling water solubility is 1.22 grams/100 mL of water. In this experiment, water solubility will be an indicator for how much boiling water to use in recrystallization, which purifies the unknown precipitate produced in the second lab. If a substance has higher water solubility in boiling water, such as acetanilide compared
20) If the solid is still not dissolved, add a tiny amount of hexane and swirl again.
Recrystallization purifies a crude product by separating the product from impurities based on solubility. The product being purified should easily dissolve in the chosen solvent at high temperatures, but not at room temperature. Impurities should dissolve in the solvent at room temperature but not at high temperatures.
Substance A and B were weighed; Substance A weighed 0.502 g and substance B weighed 0.503 g. Both substances were put into two different test tube with approximately 8 ml of DI water into the test tub. Substance A and B were stirred and B dissolved while A did not. This shows that B is soluble in water compared to A. Thus, shows that B is soluble in water than A. The reason why B is soluble in water is because it has a higher dipole moment than A. With a higher dipole moment, it shows that it is soluble in water since it is polar and the bonds were easily broken.
The product was placed in a Craig tube and several drops of hot (100°C) solvent (50% water, 50% methanol, by volume) was added and heated until all of the crystals dissolved. The Craig tube was plugged and set in an Erlenmeyer flask to cool. Crystallization was induced once the mixture was at room temperature by scratching the inner wall of the tube. It was then placed into an ice bath for ten minutes until crystallization was complete. The tube was then
Both reactants are soluble and one of the products is a solid. A soluble substances dissolves with water but an insoluble substance doesn't. In a solution, which is a homogenous mixture of two or more substances, one will have a solvent and solute. The solvent
Purpose: The purpose of this laboratory was to gain an understanding of the differences between the freezing points of pure solvent to that of a solvent in a solution with a nonvolatile solute, and to compare the two.
Solub. Or Reaction w/ hot H20: no change observed from the cool water and is soluble
The solution is then cooled and recrystallization of the solute occurs. For a solvent pair to
The recrystallization technique utilizes the ability of a compound to dissolve within a hot solvent and produce a solution. As this solution cools, the solute reforms without impurities in a crystal lattice structure.1 For this to work properly, an appropriate solution that will not dissolve the solute at low temperatures, but will at high temperatures, must be used.1 There is no single solvent that will work well for every solute’s recrystallization; different solvents are better suited for some solutes than others.2 Some impurities that do not dissolve within the solvent can be filtered out while the solution is still hot, while other impurities that readily dissolve within the solvent shouldn’t recrystallize with the pure substance (as they are not concentrated enough to
For the first lab, students worked individually to purify vanillin, but worked in pairs in order to purify an unknown. We began the process of purifying vanillin by weighing it out and dissolved in water, afterwards we placed the solution in an ice bath. After a minutes, we vacuumed out the vanillin, in order to obtain the crystals. In general, recrystallization is used to purify compounds—which was the purpose of this la . As for the unknown solid, a similar process was conducted. However, for the unknown, students had to determine the right solvent in which the unknown would dissolve in and be used for the
If the solute melts prior to the boiling of the solvent, recrystallization will not be able to occur. For example, if you wanted to purify a sample of Compound X which is contaminated by a small amount of Compound Y, an appropriate solvent would be one in which all of Compound Y dissolved at room temperature because the impurities will stay in solution and pass through filter paper, leaving only pure crystals behind. Also appropriate would be a solvent in which the impurities are insoluble at a high temperature because they will remain solid in the boiling solvent and can then be filtered out. Finally, the solvent should be volatile enough as to evaporate from the surface of the compound and be of low financial cost.
Generally, increasing temperature would cause a comparable rise in the solubility of liquid and solid solutes in liquid solvents.