Separation Of Acetylacetone

The purpose of this lab was to determine the limiting reactant in a mixture of to soluble salts and the percent composition of each substance in a salt mixture.

Experiment 55 consists of devising a separation and purification scheme for a three component mixture. The overall objective is to isolate in pure form two of the three compounds. This was done using extraction, solubility, crystallization and vacuum filtration. The experiment was carried out two times, both of which were successful.

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

3.0g of salicylic acid was weighed then 3.0mL of acetic anhydride and 6 drops of 85% H3PO4 were added to it. The mixture was warmed over a water bath for 5 minutes while stirring. After warming, 20 drops of distilled water was slowly added. 15mL of water was added then the solution was heated until it became clear. It was allowed to cool and was placed in an ice bath until the solution becomes cloudy. Using pre-weighed filter paper, the mixture was filtered and was allowed to dry in the filter paper.

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°

Experimental Method: A filtration apparatus was set up. Solid iron(III) chloride hexahydrate was dissolved in water. In a separate container, sodium acetate trihydrate (NaC2H3O2 x 3 H2O) was also dissolved in water. Sodium acetate trihydrate was then added to iron(III) chloride. 2, 4-pentanedione (C5H8O2) was dissolved in methanol; it was then added to the iron(III) chloride/sodium acetate solution. The product of this mixture was filtered, and the precipitate

Product bubbled upon addition to the hydrochloric acid; liquid turned cloudy ¡V precipitate was present; zinc sample disintegrated slowly and turned black in color.

6. Fe (NO3)3, Ferric nitrate, is much more active than ferrous. It could be identified by its reddish color and when mixed with thiocyanate, it reveals a “bloody” red color.

Part 1: Obtain some 0.200M Fe(NO3)3 solution and some 0.00020M KSCN solution. Starting from the first solution, pour and mix 8.0mL of Fe(NO3)3 solution and 2.0mL of KSCN solution into a test tube, where as the second solution has 7.0mL of Fe(NO3)3 solution and 3.0mL of KSCN solution. Continue this process until 5 test tubes have been filled. Pour

The wet, crude product was placed into the 50 mL Erlenmeyer flask. Small amounts of CaCl2 were added to dry the solution. The flask was sealed and the mixture was swirled and left to settle. Once

The next day an orange goopy textured product resulted. The extracts were then dried and combined with anhydrous sodium sulfate, then evaporated with dry air under the hood in a warm water bath. The liquid was cooled and had an initial weighing of 0.5887g. It was reweighed several minutes later with a final

The result was small white crystals, which were dry and had barely contained any moisture. The product was then dissolved in methylene chloride and dried with granular anhydrous sodium sulfate. The drying agent would have removed any water in the solution and presented a colorless solution. The solvent was evaporated and the product was collected; it had the appearance of small, white solids. Data Table 2 shows the results and calculations that were gathered after the completion of this experiment. A boiling point of the product was found to be 210℃. According to literature, the boiling of isoborneol should be 212℃. As a result, the product is most likely isoborneol. No errors had occurred during the course of the experiment, which is testified by the high yield of

To do this, a hot water bath was prepared and by placing 250 mL of deionized water into a 600 mL beaker and heating it to 70˚C using a hotplate. An Erlenmeyer flask with 70 mL of deionized water was placed into the hot water bath. When the temperature of the hot water bath was at a constant 70˚C, 0.000 g of FeCl3 and 0.000 g of FeSO4· 7 H2O were added to the Erlenmeyer flask. The flask was swirled around in order to dissolve any solid compounds before being removed from the hot water bath. 20 mL of 2.5 M NaOH was then added drop wise to the solution, so that a black precipitate formed. The solution was allowed to cool before being placed in a centrifuge for 5 minutes at 4000 rpm. The supernatant was then removed, and deionized water was poured over the precipitate to fill the centrifuge tube. Once again, the solution was centrifuged for 5 minutes at 4000 rpm, and the supernatant was removed. The remaining solid, which would ultimately harden to form clay, was removed from the centrifuge tube using a spatula and placed in a beaker to dry for 7

Dissolve the corresponding salt mostly nitrate in desired amount in double distilled water. Dissolve pure Salicylic Acid (20%) in Methanol in another beaker and Quinolin (80%) in minimum Acetic Acid in the third one. Prepare separate solution of NaOH by dissolving NaOH pellets in double distilled water in the fourth beaker. Add solution of Quinolin (80%) to Salicylic Acid (20%) solution and then add NaOH solution to the mixed solutions. The solution of NaOH is needed to maintain basicity in the solution (i.e pH >7). Precipitate is obtained which was then filtered with the help of filter paper. The filtrate was dried under the lamp for several hours to drive away the moisture and used for photoluminescence measurements. Photoluminescence measurements

One milliliter of sodium chromate was pipetted into a small test tube, then one milliliter of zinc sulfate was added to the tube and mixed. The students then conducted a pH test by using a glass stirring rod and placing a single drop of the solution onto the pH paper provided. Afterwards, up to five drops of sodium hydroxide were added to the test tube to neutralize the solution. The pigment was then filtered. Filtering was performed by placing a round piece of filter paper in the funnel. The vacuum was then turned on and water was added to the filter paper in order to prevent pigment leakage. The pigment was then added to the funnel and water was used to clean off the crystals. The chrome yellow pigment was then placed on another sheet of filter paper for