ࡱ> 7A6e%`  bjbj"x"x 9@@ N N N N j . :  hdWa"WW ???WF  ?W??:, ~ `œ< N : 0. zRzz<>,?$9).WWWW* $*  Simple Distillation  INCLUDEPICTURE "http://designer-drug.com/pte/12.162.180.114/dcd/chemistry/equipment/pictures/zubrick098.gif" \* MERGEFORMATINET  For separation of liquids boiling below 150C at 1 atm from Nonvolatile impurities. Another liquid boiling 25C higher than the first liquid. They must dissolve in each other. The Three-Way Adapter If there is any one place your setup will fall apart, here it is When you set up the jointware, it is important that you have all the joints line up. This is tricky, since, as you push one joint together, another pops right out. If you're not sure, call your instructor to inspect your work. Remember, all joints must be tight! Grease all ground glassware joints as you assemble the apparatus. Clamping  EMBED Word.Picture.8  It is also wise to use some type of clamps to connect the various pieces of the distillation apparatus together. Be sure to use the clips to attach the vacuum adaptor and the Claisen tube and the distillation adaptor. The Distilling Flask  INCLUDEPICTURE "http://designer-drug.com/pte/12.162.180.114/dcd/chemistry/equipment/pictures/zubrick099.gif" \* MERGEFORMATINET  Choose a distilling flask carefully. If it's too big, you'll lose a lot of your product. If it's too small, you might have to distill in parts. Don't fill the distilling flask more than half full. Less than 1/3 full and you'll probably lose product. More than 1/2 full and you'll probably have undistilled material thrown up into the condenser (and into your previously clean product). Fill the distilling flask with the liquid you want to distill. You can remove the thermometer and thermometer adapter, fill the flask using a funnel, and then put the thermometer and its adapter back in place. Put in a boiling stone if you haven't already. These porous little rocks promote bubbling and keep the liquid from superheating and flying out of the flask. This flying around is called bumping. Never drop a boiling stone into hot liquid, or you may be rewarded by having your body soaked in the hot liquid as it foams out at you. Make sure all the joints in your setup are tight. Start the heat s-l-o-w-l-y until gentle boiling beg-ins and liquid starts to drop into the receiving flask at the rate of about 10 drops per minute. This is important. If nothing comes over, you're not distilling, but merely wasting time. You may have to turn up the heat to keep material coming over. Never distill the still pot to dryness in this or any distillation. The Thermometer Make sure the entire thermometer bulb is below the side arm of the three-way adapter. If you don't have liquid droplets condensing on the thermometer bulb, the temperature you read is nonsense. Keep a record of the temperature of the liquid or liquids that are distilling. It's a check on the purity. Liquid collected over a 2C range is fairly pure. The Condenser Always keep cold water running through the condenser, enough so that at least the lower half is cold to the touch, Remember that water should go in the bottom and out of the top Before turning the water flow on, check the hose connections carefully to ensure that they are secure and will not pop off. An extra margin of security can be gained by twisting wire around the hose connections. The water flow is adjusted so there is a slow, constant flow of cold water to the condenser. You really only need a trickle, more than that will cause the hoses to pop off, spray your neighbors, and cause a flood. The Receiving Flask and Vacuum Adaptor The receiving flask should be large enough to collect what you want. You may need several, and they may have to be changed during the distillation. Standard practice is to have one flask ready for what you are going to throw away and others ready to save the stuff you want to save. Typically, the liquid should drip into the receiving flask at a rate of about 10 drops per minute. If the rate of distillation is too rapid, the heat applied to the distillation flask must be decreased. With too rapid a rate, the measured boiling point is likely to be inaccurate and the purity of the distilled liquid will be compromised. The system is open to the atmosphere via the vacuum adaptor. This apparatus is being heated, and you should never heat a closed system. If the liquid being collected has a low boiling point, it is good practice to cool the receiving flask with a cold water bath. The Ice Bath Why everyone insists on loading up a bucket with ice and trying to force a flask into this mess, I'll never know. How much cooling do you think you're going to get with just a few small areas of the flask barely touching ice? 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