Experiment 5: Separating Ferrocene and Acetylferrocene by Adsorption Column Chromatography
AIM
The primary goal of this experiment is to separate ferrocene and acetylferrocene using adsorption column chromatography. Additionally, a dry pack method with a micro scale column will be implemented, and the percent recovery for each compound will be computed.
TABLE OF PHYSICAL PROPERTIES AND HAZARDS WITH STRUCTURES
Ferrocene: -
Physical Property: Solid
Molecular Weight: 186.04 g/mole
Boiling Point: 249 °C
Melting Point: 173.5 °C
Solubility: insoluble in cold water
Hazards: This compound can be dangerous if it comes into contact with one’s skin, eyes or if it is ingested or inhaled.
Structure:
Acetylferrocene: -
Physical …show more content…
Use a micro spatula to obtain a sample of sand, and then line a ruler up against the pipet to add 5mm of the sand. Also, tap the pipet to ensure that the sand is compact and has an even top layer.
6. Use the ruler method in step 4, and add 5cm of silica gel to the pipet and tap to ensure there is an even layer.
7. Weight out and add approximately 0.02 g of the 50/50 mixture of ferrocene and acetylferrocene, and add it to the pipet while repeating the tapping method.
8. Repeat Step 4.
9. The flask labeled “hexane” is filled with approximately 25 ml of hexane, and the one labeled “organic solvent” is placed under the column in order to collect the hexane.
10. Use a pipet to slowly add 1ml of hexane in increments to avoid any overflowing.
11. Keep adding and collecting the hexane until the yellow ferrocene reaches the bottom of the column bed, and immediately start to collect it in the sample vial labeled “F”
12. After all of the ferrocene has been collected, place the flask labeled “organic solvent” under the column
13. Repeat Steps 9 through 12, but instead replace hexane with ethyl acetate, and use the sample vial labeled “AF” to collect the orange acetylferrocene.
14. Lastly, the two sample vials are to be evaporated using the rotary evaporator, and then has to be weighed and recorded. …show more content…
Flow Chart: RESULTS
Table 1.1 separations of ferrocene and acetylferrocene
Compound Empty Vial (g) Vial + Compound (g) Final Weight (g) Percent Recovery (%)
Ferrocene 9.564 11.011 9.720 88.3
Acetylferrocene 9.620 10.348 9.61 93
A description of the physical properties of the compounds has been explained in the observation section of this laboratory report.
CONCLUSIONS
My laboratory partner and I were able to successfully separate the ferrocene and acetylferrocne by using the method of adsorption column chromatography. Since both of the compounds are aromatic organometallic, ferrocene and acetylferrocene both showed up as yellow and orange bands in the pipet respectively. The separation of both compounds was successful due to the polarity of the eluent being controlled. Some of the factors that may have contributed to the percent recovery being less than 100 percent are the lack of collect every minute amount of the two compounds. Also, some of the compounds could have been lost through the Erlenmeyer flasks or maybe some of it was lost through the rotary
AIM
The primary goal of this experiment is to separate ferrocene and acetylferrocene using adsorption column chromatography. Additionally, a dry pack method with a micro scale column will be implemented, and the percent recovery for each compound will be computed.
TABLE OF PHYSICAL PROPERTIES AND HAZARDS WITH STRUCTURES
Ferrocene: -
Physical Property: Solid
Molecular Weight: 186.04 g/mole
Boiling Point: 249 °C
Melting Point: 173.5 °C
Solubility: insoluble in cold water
Hazards: This compound can be dangerous if it comes into contact with one’s skin, eyes or if it is ingested or inhaled.
Structure:
Acetylferrocene: -
Physical …show more content…
Use a micro spatula to obtain a sample of sand, and then line a ruler up against the pipet to add 5mm of the sand. Also, tap the pipet to ensure that the sand is compact and has an even top layer.
6. Use the ruler method in step 4, and add 5cm of silica gel to the pipet and tap to ensure there is an even layer.
7. Weight out and add approximately 0.02 g of the 50/50 mixture of ferrocene and acetylferrocene, and add it to the pipet while repeating the tapping method.
8. Repeat Step 4.
9. The flask labeled “hexane” is filled with approximately 25 ml of hexane, and the one labeled “organic solvent” is placed under the column in order to collect the hexane.
10. Use a pipet to slowly add 1ml of hexane in increments to avoid any overflowing.
11. Keep adding and collecting the hexane until the yellow ferrocene reaches the bottom of the column bed, and immediately start to collect it in the sample vial labeled “F”
12. After all of the ferrocene has been collected, place the flask labeled “organic solvent” under the column
13. Repeat Steps 9 through 12, but instead replace hexane with ethyl acetate, and use the sample vial labeled “AF” to collect the orange acetylferrocene.
14. Lastly, the two sample vials are to be evaporated using the rotary evaporator, and then has to be weighed and recorded. …show more content…
Flow Chart: RESULTS
Table 1.1 separations of ferrocene and acetylferrocene
Compound Empty Vial (g) Vial + Compound (g) Final Weight (g) Percent Recovery (%)
Ferrocene 9.564 11.011 9.720 88.3
Acetylferrocene 9.620 10.348 9.61 93
A description of the physical properties of the compounds has been explained in the observation section of this laboratory report.
CONCLUSIONS
My laboratory partner and I were able to successfully separate the ferrocene and acetylferrocne by using the method of adsorption column chromatography. Since both of the compounds are aromatic organometallic, ferrocene and acetylferrocene both showed up as yellow and orange bands in the pipet respectively. The separation of both compounds was successful due to the polarity of the eluent being controlled. Some of the factors that may have contributed to the percent recovery being less than 100 percent are the lack of collect every minute amount of the two compounds. Also, some of the compounds could have been lost through the Erlenmeyer flasks or maybe some of it was lost through the rotary