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Lecture 5

CHEM 235 Lecture Notes - Lecture 5: Separatory Funnel, Diethyl Ether, Sodium Sulfate


Department
Chemistry
Course Code
CHEM 235
Professor
Dana Zendrowski
Lecture
5

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Lab 6 (PART 1): test tubes, spatula, separatory funnel, glass filtering funnel, glass rod, 100 ml beaker (2),
50 ml E.F(2), 125 ML E.F., RB flasks, fluted filter paper
1. Small test tubes containing 2-3 ml of each solvent, anf few ground crystals for Test on Mixture
2. Weigh out 1.3 -1.4 g of sample , pour it in 100 ml beaker
3. Dissolve them in 30 ml/NEEDED diethyl ether and pour it into separatory funnel
4. Rinse the beaker with 5 ml ether and add it to separatory funnel
5. Add 10 ml of 10% NaOH/ 5% NaHCO3 in the solution, shake it, extract lower layer in a 100 ml
beaker
6. Repeat number 5 twice
7. Wash the solution in the funnel with 10 ml of water
8. Add the wate wash to the aueous etats, lael the eake acid fatio
9. Pour ether layer out of the top of separatory funnel into 50 ml Erlenmeyer flask and label
eutal fatio
10. Rinse the separatory flask with 5 ml of diethyl ether and pour it out of the funnel into the E.F
11. add anhydrous sodium sulfate(drying agent) in the solution, add cork 6, swirl until the liquid is
white in color, if clumps visible, add more drying agent
12. dry at least 10 minutes with the cork on
13. add 10% HCl in the acid fatio, stir it with the glass rod and use litmus paper to identify if its
acidic(red). Add HCl until its acidic. This is the acid fatio.
14. Add 15 ml diethyl ether in the separatory funnel, add the base fraction, and shake it. Extract the
top layer i 5 l EF, ae is acid fatio.
15. Repeat adding 15 ml diethyl ether and the extraction twice
16. Rinse funnel with 5 ml of ether and add it to acid fraction
17. Dry the solution with anhydrous sodium sulfate for 10 minutes. Cork 12
18. Preweigh 50 and 100 ml RB flasks, and record
19. Use glass fuel ad fluted filte pape to filte off dig aget fo the eutal fatio in 50
ml RB flask
20. RB flask should never be more than half full; too Much solution transfer some in EF
21. Use rotary evaporator to evaporate ether
22. Use glass fuel ad fluted filte pape to filte off dig aget fo the acid fatio i  l
RB flask
23. Pour some solution in the EF, RB flask should be half full only
24. Use rotary evaporator to evaporate ether
25. Weight the RB flask containing dry sample and do percent recovery for both neutral and basic
compounds
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