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BananaOilProcNotesFall04 - 8 Reflux for prescribed time...

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Banana Oil Procedure Notes Be careful with concentrated acids! 1) We are not using a calcium chloride drying tube on top of the condenser. 2) Isopentyl alcohol is also called isoamyl alcohol. 3) We are not using a calibrated pipette. One Pasteur pipette load of sulfuric acid is close enough to 1 ml. 4) Use a Teflon boiling chip instead of boileezer. 5) The slender column is the condenser, the fat one is the distiller. 6) Connect cooling water to bottom fitting on condenser, run hose from the top fitting, down into the sink. Adjust flow so that water flow is constant, and falls straight down if you hold the hose horizontally. Set-up distillation apparatus in the hood and connect rubber tubing to the green nozzle labeled CW (cold water) and let water flow out into drain. See page 734 in textbook for diagram of apparatus. 7) Adjust temperature with voltage regulator so that vapor is condensing approximately 1/3 of the way up the column.
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Unformatted text preview: 8) Reflux for prescribed time period. Record the appearance change in the mixture. 9) Do not transfer the boiling chip into the separatory funnel on the extraction step. 10) Be careful with separatory funnel (especially with bicarbonate wash). The rapid buildup of gas may cause the top to burst off while inverted. When beginning the extraction, invert and vent IMMEDIATELY, then vent every few seconds until the acid/base reaction subsides. 11) While distilling, note the temperature “range”, not point, over which you collect your ester. Drip rate should be no faster than 1 drop per two seconds if you are heating properly. Make sure cooling water flows up hill again. 12) We will omit the spectroscopy and boiling point determination portions of the experiment. 13) You will neutralize your aqueous waste with solid baking soda in the hood. 14) This is a long lab--- be prepared so it will run smoother and faster....
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