8. Attach one length of rubber tubing to the lower condenser jacket sidearm.

The other end of the rubber tubing should be placed over the nozzle of the lab sink. 9. Attach the second length of rubber tubing to the upper condenser jacket sidearm. The other end of the rubber tubing should be placed into the sink to allow the condenser water to drain. 10. Place a beaker underneath the spout of the condenser to collect the distillate. 11. Attach a Bunsen burner to a gas jet, and adjust the tubing so that the burner sits safely beneath the distilling flask.

Equipment Needed

Beaker (1 or more, depending on the number of components in the mixture) Liebig Condenser (1) Thermometer (1) Distilling Flask (1) Utility Clamps (2, minimum) Ring stand (2) Rubber tubing (2, 16"-24" length each) Bunsen burner and tubing (1) Rubber stopper or cork, one-hole (2)

Distillation is a method of separating or purifying liquids based on their different boiling points. If you don't wish to construct the distillation apparatus and can afford it, you can buy a complete set up. That can get expensive, so here is an example of how to set up a distillation apparatus from standard chemistry equipment. You can customize your setup based on what you have on hand. Distillation Equipment

Setup 1. Attach a utility clamp to each ring stand. 2. Carefully insert the flask sidearm into a onehole stopper or cork. Use a twisting motion with gentle pressure. Protect your hands with paper towels, and use water or glycerin to lubricate the sidearm. 1 cm or less of the sidearm should stick out of the stopper when finished. 3. Attach the distilling flask to one of the mounted utility clamps. Place the jaws of the clamp below the sidearm of the flask. Adjust the height of the clamp and flask to leave enough room for the Bunsen burner. 4. Carefully insert a thermometer into a one-hole stopper or cork. Use a twisting motion with gentle pressure. Protect your hands with paper towels, and use water or glycerin to lubricate the thermometer. Place the stopper in the opening of the flask's neck. Adjust the level of the thermometer so that the bulb is the same height as the flask sidearm. 5. Attach the Liebig condenser to the second mounted utility clamp. The angle of the clamp will need to be adjusted so that it matches the angle the flask sidearm makes with the flask neck. 6. Adjust the height of the condenser utility clamp and move the condenser ring stand so that the opening of the condenser column is even with the sidearm stopper. 7. Insert the sidearm stopper into the opening of the condenser column and ensure that there is a snug fit.

2 Erlenmeyer flasks 1 1-hole stopper that fits a flask 1 2-hole stopper that fits a flask some plastic tubing short lengths of glass tubing cold water bath (any container that can hold both cold water and a flask) boiling chip hotplate thermometer (optional) If you have them, two 2-hole stoppers are ideal because then you can insert a thermometer into the heated flask. This is helpful and sometime necessary to control the temperature of the distillation. Also, if the temperature of the distillation suddenly changes, this usually indicates one of the chemicals in your mixture has been removed. Set Up the Distillation Apparatus 1. The liquid you are distilling goes into one beaker, along with a boiling chip. 2. This beaker sits on the hot plate, since this is the liquid you will be heating. 3. Insert a short length of glass tubing into a stopper. Connect it to one end of a length of plastic tubing.

4. Connect the other end of the plastic tubing to a short length of glass tubing inserted into the other stopper. The distilled fluid will pass through this tubing to the second flask. 5. Insert a short length of glass tubing into the stopper for the second flask. It is open to the air to prevent pressure buildup inside the apparatus. 6. Place the receiving flask in a large container filled with ice water. Vapor passing through the plastic tubing will condense immediately when it comes into contact with the cooler air of the receiving flask. 7. It's a good idea to clamp down both flasks to help keep them from tipping over by accident.

thermal shock to the glassware. As mentioned in the section on flowing water, the hoses must be connected tightly enough to the condenser that they will not come loose if the water pressure should increase during the experiment. Usually this means that something like copper wire is twisted around the tubing at the joint to prevent it from coming away. The flow of water must be sufficient to accomplish condensation without being so fast as to cause undue hose pressure or splashing of outflow water, remembering that flow rates can change during the day after they have initially been set. The distillation flask should preferably be a round-bottomed one rather than a flat-bottomed one for smoothness of boiling. The flask should never be more than half-filled with the liquid mixture to be distilled. Greater filling leads to bubbles and sometimes foaming that is constricted in the narrowing part of the flask and gets out of control. To make boiling smoothest, boiling chips or tubes should be added to the liquid in the distillation flask before heating has begun. It is very important not to add chips or tubes to heated liquid as it may suddenly begin to boil and eject hot liquid out onto the operator. The chips are generally made of sharp pieces of broken ceramic or hard plastic. Tubes are usually of the capillary type with both ends open. Heating the distillation flask requires care. The liquids being distilled are often flammable so that flame is not the preferred heat source. Heating mantles or sand baths are good sources of heat to conform to the round-bottomed flasks. Care must be taken not to let any vapors near the control switches that may spark when opening and closing. Doing the distillation inside a hood is a good practice. One last word of caution about the apparatus is in order. There have been cases where the operators decided to make the connection between the condenser and the receiving vessel a tight one using a stopper or standard taper connection. This must NOT be done as it creates a completely sealed system. When the distillation flask is heated and vapors begin to rise they will expand and create a pressure in such a sealed system that will inevitably blow the joints apart. This generally causes vapors to escape into the surrounding room (or hopefully hood) if not the glassware to be broken. Always allow for a pressure relief opening in the distillation system between the condenser and the receiving vessel. Note in the diagram above the glass connector where the drops are falling is NOT sealed but is only loosely in the receiving flask. What's distillation used for? Distillation is a laboratory technique used for separating and purifying liquids. How does distillation work?

Distillation is a common operation in many laboratories for the purpose of separating and/or purifying components of a liquid mixture. The apparatus used consists of three major parts: distillation flask (or pot) to heat the mixture and volatilize the components, a condenser to cool the vapors back to liquid state, and a collection vessel. Many of the hazards associated with the distillation process have been discussed in previous sections (glassware, flowing water, heating devices). However, the importance of the procedure is such that it is advisable to collect the warnings in this one place to make sure nothing goes unnoticed. The apparatus is usually made of glass and therefore subject to breakage. All components of the distillation apparatus should be secured to a stable stand or rack to prevent it from falling over. All the glassware, particularly the part to be heated, should be checked for cracks prior to use. Connections between the glass parts may involve rubber or cork stoppers but in more modern apparatus standard taper connections are used. If stoppers are used, it must be known that the hot vapors will not react with the rubber or cork and thus contaminate the products. If standard taper connections are used, any lubricant used to make tight seals must also not react, melt or evaporate and contaminate the product. The condenser must generally be connected to a source of running water to provide cooling for the vapors. The proper method is to connect the input hose to the condenser at the end furthest from the heated flask and the outflow hose nearest the heated flask. This prevents the hottest vapors from contacting the coldest water and creating a large

Distillation works by exploiting the different boiling temperatures of liquids. To separate two or more liquids by distillation, you first heat them in a flask. The more volatile liquid (the liquid with the lower boiling point) will typically evaporate first and the

vapor will pass into a condensing column, where it can revert into a liquid (condense) on the cool glass where it trickles into a collection flask. Heating further will cause the less volatile liquids to evaporate and distill at higher temperatures. The two main kinds of distillation are simple distillation and fractional distillation, and both are used widely. What is simple distillation? A simple distillation apparatus consists of a boiling flask (round-bottom flask) attached to an adapter holding a thermometer (to determine the boiling temperature of the liquid). The adapter connects to a condenser into which cold water is constantly passed through. The condenser leads into a collection flask for the purified liquid. What is fractional distillation? Fractional distillation is essentially the same as simple distillation except that a fractionating column is placed between the boiling flask and the condenser. The fractionating column is usually filled with glass or plastic beads. These beads improve the separation between the liquids being distilled. The reason that fractional distillation gives better separation between the liquids is because the glass beads in the fractionating column provide "theoretical plates" on which the refluxing liquid can condense, re-evaporate, and condense again, essentially distilling the compound over and over. The more volatile liquids will tend to push towards the top of the fractionating column, while lower boiling liquids will stay towards the bottom, giving a better separation between the liquids. Of course, the more theoretical plates that you add to a column (the more surfaces or beads), the longer the distillation will take (typically), and the more energy required to keep reevaporating liquid in the fractionating column (this is more of a concern in industrial distillations than in an academic lab where energy cost is not a major cause for worry). So, simple or fractional? The choice of whether to use fractional distillation or simple distillation depends on the two liquids being separated. Typically, using simple distillation is preferrable because the apparatus is, well, simpler, and a simple distillation typically goes faster than a fractional distillation (and requires less energy). On the other hand, fractional distillation gives better separation between the liquids. The choice of whether to use simple or fractional distillation, then, depends usually on the difference in boiling temperatures between the two liquids. If there is a large difference in the boiling points (>70oC)between the two liquids then simple distillation is probably the best option. On the other hand, if there is only a small temperature difference between the two liquids a fractional distillation is the preferrable option. Simple distillation Advantages simpler setup than fractional Fractional distillation

times consumes less energy than fractional distillation requires the liquids to have large boiling point differences (>70oC)

distillation can more readily purify complex mixtures than simple distillation

more complicated setup than simple distillation

Disadvantages gives poorer takes longer for separation than liquids to distill fractional distillation consumes more energy than only works well simple distillation with relatively pure liquids separating relatively pure liquids with Best used for: large boiling differences or liquids with solid impurities separating complex mixtures of liquids with smaller boiling point separations.

The separation or purification of liquids by vaporization and condensation is a very important step in one of our oldest professions, The word "still" lives on as a tribute to the importance of organic chemistry. There are two important points here.

1. Vaporization. Turning a liquid to a vapor. 2. Condensation. Turning a vapor to a liquid.

Remember these. They show up on quizzes. But when do I use distillation? That is a very good question. Use the guidelines below to pick your special situation, and turn to that section. But you should read all the sections anyway.

1. Class 1: Simple distillation. Separating

much better separation between liquids faster distillation than simple

liquids boiling below 150C at one atmosphere (1 atm) from a. Nonvolatile impurities. b. Another liquid boiling at least 25C higher than the first. The liquids should dissolve in each other. 2. Class 2: Vacuum distillation. Separating liquids boiling above 150C at 1 atm from a. Nonvolatile impurities. b. Another liquid boiling at least 25C higher than the first. They should dissolve in one another. 3. Class 3: Fractional distillation. Separating liquid mixtures, soluble in each other, that boil at less than 25C from each other at 1 atm. 4. Class 4: Steam distillation. Isolating tars, oils, and other liquid compounds that are insoluble, or slightly soluble, in water at all temperatures. Usually, natural products are steam distilled. They do not have to be liquids at room temperatures. (For example, caffeine, a solid, can be isolated from green tea.)

CLASS 1: SIMPLE DISTILLATION For separation of liquids boiling below 150C at 1 atm from 1. Nonvolatile impurities. 2. Another liquid boiling 25C higher than the first liquid. They must dissolve in each other. SOURCES OF HEAT If one of the components boils below 70C and you use a Bunsen burner, you may have a hard time putting out the fire. Use a steam bath or a heating mantle. Different distillations will require different handling. All the distillations always require heating. This goes for enlightenment on the use of boiling stones and clamps as well. 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. Remember, All joints must be tight! THE DISTILLING FLASK 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. If you're doing a fractional distillation with a column (a Class 3 distillation), you should've filled the flask before clamping the setup. (Don't ever pour your mixture down a column. That'll contaminate everything!) You'll just have to disassemble some of the setup, fill the flask, reassemble what you've taken down, and pray that you haven't knocked all the other joints out of line. 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. THE THERMOMETER ADAPTER Read all about it. Ways of having fun with thermometer adapters have been detailed. THE UBIQUITOUS CLAMP A word about clamps. Use! 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. Note the similarity of this range with that of the melting point of a pure compound. 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. Also, the water pressure in the lab may change from time to time and usually goes up at night, since little water is used then. So, if you are going to let condenser cooling water run overnight, tie the tubing on at the condenser and the water faucet with wire or something. And if you don't want to flood out the lab, see that the outlet hose can't flop out of the sink. THE VACUUM ADAPTER It is important that the tubing connector remain open to the air; otherwise, the entire apparatus will, quite simply, explode. Warning: Do not just stick the vacuum adapter on the end of the condenser and hope that it will not fall off and break. This is foolish. I have no sympathy for anyone who will not use clamps to save their own breakage fee. They deserve to pay. THE RECEIVING FLASK 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. 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? Get a suitable receptacle-a large beaker, enameled pan, or whatever. It should not leak. Put it under the flask. Put some water in it. Now add ice. Stir. Serves four. Ice bath really means ice-water bath. THE DISTILLATION EXAMPLE Say you place 50 mL of liquid A (bp. 50C) and 50 mL of liquid B (bp 100C) in a 250 mL R.B. flask. You drop in a boiling stone, fit the flask in a distillation setup, and turn on the heat. Bubbling starts, and soon droplets form on the thermometer bulb. The temperature shoots up from room temperature to about 35C, and a liquid condenses and drips into the receiver. That's bad. The temperature should be close to 50C. This low-boiling material is the forerun of a distillation, and you won't want to keep it. Keep letting liquid come over until the temperature stabilizes at about 49C. Quick! Change receiving flasks now! The new receiving flask is on the vacuum adapter, and the temperature is about 49C. Good. Liquid comes over, and you heat to get a rate of about 10 drops per minute collected in the receiver. As you distill, the temperature slowly increases to maybe 51C and then starts moving up rapidly. Here you stop the distillation and change the receiver. Now in one receiver you have a pure liquid, bp. 49-51C. Note this boiling range. It is just as good a test of purity as a melting point is for solids. Always report a boiling point for liquids as routinely as you report melting points for solids. The boiling point is actually a boiling range and should be reported as such: "bp. 49-51C" If you now put on a new receiver, and start heating again, you may discover more material coining over at 50C! Find that strange? Not so. All it means is that you were distilling too rapidly and some of the low-boiling material was left behind, It is very difficult to avoid this situation, Sometimes it is best to ignore it, unless a yield is very important. You can combine this "new" 50C fraction with the other good fraction. For liquid B, boiling at 100C, merely substitute some different boiling points and go over the same story.

THE DISTILLATION MISTAKE OK, you set all this stuff up to do a distillation. Everything's going fine. Clamps in the right place. No arthritic joints, even the vacuum adapter is clamped on, and the thermometer is at the right height. There's a bright golden haze on the meadow, and everything's going your way. So, you begin to boil the liquid. You even remembered the boiling stone, Boiling starts slowly, then more rapidly. You think, "This is it!" Read that temperature, now. Into the notebook: "The mixture started boiling at 26C." And you are dead wrong. What happened? Just askIs there liquid condensing thermometer bulb?? No! on the

So, congratulations, you've just recorded the room temperature. There are days when over half of the class will report distillation temperatures as "Hey I see it start boiling now" temperatures. Don't participate. Just keep watching as the liquid boils. Soon, droplets will condense on the thermometer bulb. The temperature will go up quickly, and then stabilize. Now read the temperature. That's the boiling point. But wait! It's not a distillation temperature until that first drop of liquid falls into the receiving flask.

Theory: Distillation Distillation is a purification technique. It can be used for the separation of a low boiling solvent from a solid

or a high boiling liquid. The liquid vaporizes in one vessel (the distillation pot) and then condenses into another vessel (the receiving flask). Heat Sources:

When no more solvent distilled over, the heating mantle was slowly lowered and the apparatus allowed to cool before disassembly.

Practical Lab Tips Steam Bath - Use with flammable liquids that have a boiling point below 100 oC. Heating Mantle with Powermite - Use with round bottom flasks during distillation or reflux. The Powermite allows heat regulation. Hot Plate - Use with Erlenmeyer flasks containing non-flammable or high boiling liquids. Can also be used with beakers containing water (for a water bath). Boiling Point: Boiling point is the temperature at which the vapor pressure of a liquid is equal to that of the surrounding atmosphere. Boiling point varies with atmospheric pressure and is corrected to the temperature that would be observed at sea level (760 Torr). The higher the altitude, the lower the atmospheric pressure and the lower the boiling point. Boiling point is measured during distillation when the temperature is constant (at the stillhead). Corrected boiling point can be measured using a nomograph or the following equation: Boiling Point Correction Factor = [(760 torr atmospheric pressure) / 10 torr x 0.5 oC] Corrected Boiling Point = Observed Boiling Point + Correction Factor Typical Experiment Student A left approximately 20mL of a liquid mixture for his partner, Student B, to work up. Student B was to remove and identify the solvent as well as retain the residue and distillate. Student B decided to use simple distillation to remove the solvent. He placed a lab jack in position and set up a heating mantle with a Powermite control. He clamped the distillation flask in place and added boiling stones followed by his unknown liquid. A stillhead was then attached and a thermometer was inserted into the thermometer adapter. The receiving flask was clamped in position and the condenser was connected between the receiving flask and distillation flask. Student B then attached the water tubing to the condenser and turn the water tap on full. The tubing popped off and sprayed the student's TA (who was not impressed). The student reconnected the tubing and this time used the hose clamps and turned on the water tap slowly. The student set the Powermite to 25 and after a few minutes, the liquid in the distillation flask began to boil. The solvent began to boil and the temperature of the distillate was observed to be 38 oC at ~700 torr. When connecting the water tubing to your condenser, remember that water enters from the bottom of the condenser and exits from the top. Add boiling stones to your distillation flask BEFORE you start heating. Distillation is complete when: a) no more liquid collects in the receiving vessel, b) when the temperature of the thermometer starts to drop or c) when the distillation flask is empty. Q: When using the water condenser, which hose connector is water-in and which is water-out? Water goes in from the BOTTOM of the condenser. Q: Why does it matter whether the water enters the condenser at the top or from the bottom? If water enters from the bottom of the condenser, it will always be completely filled with cold water which ensures efficient cooling. During distillation, vapors are formed in the heated distillation flask. The condenser cools these vapors condensing them back to liquid droplets that flow down the condenser into the receiver flask. A completely filled condenser provides maximum cooling therefore allowing for maximum recovery of the purified liquid during distillation. Q: How fast should the water run through the condenser? A continuous flow of water through the condenser is necessary; however, the lower the flow rate, the lower the pressure and the lower the chance of having the tubing pop off (resulting in you spraying yourself or others). Q: How far down the stillhead should the thermometer bulb be placed when setting up the distillation apparatus? The mercury bulb of the thermometer should be positioned so that vapors condense readily on it. The tip of the bulb should be in line with the lowest part of the connecting tube of the stillhead. Q: How do you know when distillation is complete? Distillation is complete when: a) you notice a drop in temperature, b) no more distillate is being formed or c) the distillation pot is empty. Q: Why are no drops coming over eventhough the distillate is boiling? There could be two reasons for this:

If this happens at the beginning of the distillation, there is insufficient energy input to cause adequate vaporization of the liquid. In this case, you should increase the heat. If this happens at the end of the distillation, almost all of the low boiling liquid has been removed. Solvent vapors trapped in the boiling stone pores will continue to be an ebullition source, causing bubbling. Q: Can I use a bunsen burner for reflux and distillation? It is safer to use a heating mantle with a Powermite control for flammable vapors. The Powermite also makes it easier to control the temperature. Q: When setting up the distillation apparatus, can I use an Erlenmeyer flask for the receiving flask? Yes, but there are less organic vapors if you use a small round bottom flask. Q: How much does boiling point vary with atmospheric pressure? For most organic liquids, there is a decrease of 0.5 oC with every 10 torr difference from 760 torr Q: If the atmospheric pressure is 695 torr today, does that mean the actual boiling point of this liquid is listed in the literature at a higher value than the temperature I saw, even after I corrected the temperature for my thermometer? Yes. Boiling points are usually recorded as the temperature at 760 torr. Given that, observed boiling point is lowered by 0.5 oC for every 10 torr difference below 760 torr. This means that at 695 torr, the boiling point of your liquid is actually 3.3 oC higher than the temperature you observed during distillation. Distillation is probably the most common technique for purifying organic liquids. In simple distillation, a liquid is boiled and the vapors work through the apparatus until they reach the condenser where they are cooled and reliquify. Liquids are separated based upon their differences in boiling point. Two important things to note: 1) the tip of the thermometer must be correctly positioned slightly below the center of the condenser to accurately reflect the temperature of the vapors (see above left) and 2) the water supply should be connected to the lower port in the condenser and the drainage tube connected to the upper (in the picture on the right the right tube is connected to the water supply and the red tube is a drainage tube). Also be sure to use the thin-walled tubing and not the heavy walled vacuum tubing. Be very careful that your water lines do not come in direct contact with your hot plate, as the lines could melt resulting in a flood. Be sure to clamp both the round bottom boiling flask and the collection tube. Knocking over your collection tube at the end of the experiment if VERY frustrating. Below is a diagram of assembly: Generally, boiling stones will be added to the boiling flask to ensure even

boiling. It is also wise to use some type of clamps to connect the various pieces of the distillation apparatus together. For low boiling liquids, enough heat may be provided simply by resting your flask on the hot plate (as shown above). You can also insulate your boiling flask and Claisen adaptor with aluminum foil. For higher boiling liquids it may be necessary to use an oil or sand bath to reach higher temperatures. The setup for a fractional distillation is very similar to that for simple distillation. The only difference is the addition of a fractional distillation column, usually packed with some material of high surface area that produces a more efficient separation than the simple distillation. The same advice regarding the thermometer placement, clamping, and hook-up of the water tubes in the simple distillation also apply to the fractional distillation. As this apparatus is larger, practice additional caution to be sure that no glassware is broken or product loss. The choice whether to use the simple or the fractional setup will depend on the compounds that you are trying to separate. Obviously, the simple distillation setup is simpler and the distillation generally will be quicker than the fractional. However, the fractional setup is more efficient at separating liquids with fairly similar boiling points and at times is required.

Begin with a round-bottom flask. This is one of the most critical pieces of glassware in the assembly, since it will hold the liquid to be distilled. You don't want it to fall and break because you would lose your compound and possibly spill a hazardous chemical. To secure your setup, you will need a small threepronged clamp, two ring stands, and a ring clamp. Place the ring clamp and three-pronged clamp on the ring stand. The ring clamp goes on the bottom and will hold the heat source, either a steam bath (no longer used in the organic labs) or a heating mantle. Secure the round-bottom flask to the ring stand using the three-pronged clamp. The next item to be added is the Y-adaptor. The Y-adaptor sits on top of the round-bottom flask. The next item to be added, thecondenser , will secure the Y-adaptor to the system. You will also need a Keck clip and aversatile clamp. Connect the condenser to the Y-adaptor and secure the connection with a Keck clip. Secure the condenser to the ring stand with a versatile clamp. The next items you will need are a vacuum adaptor and another Keck clip. Connect the vacuum adaptor to the condenser and secure the connection with a Keck clip. Add a couple of boiling chips to the round-bottom flask by dropping them down through the Y-adaptor. Place a stemmed funnel into the top of the Y-adaptor and pour the liquid to be distilled through it so that it

goes into the round bottom flask. The flask should be between 1/2 full and 2/3 full. When done, remove the funnel. an Erlenmeyer flask has been placed under the vacuum adaptor. This is the receiving flask. A beaker, vial or graduated cylinder could also be used. In a vacuum distillation, a round bottom flask is used as the receiving flask, and it is securely attached with either a clamp or a yellow clip. The next items to be added are the thermometer adaptor and thermometer. The thermometer is always added last because it is large and susceptible to breakeage. Here is all the glassware properly assembled. The thermometer and thermometer adaptor are connected on top of the Y-adaptor. Note the correct placement of the thermometer - this is vital for correct measurement of boiling point. The collection flask has been temporarily removed to protect it during the addition of the heat source, which could cause an unsecured flask to fall and break. Collect two pieces of Tygon tubing for the condenser. If you are using a steam bath for the heat source, you will need four lengths. Place the heat source on the ring under the roundbottom flask. Adjust the height of the apparatus as necessary. Connect two pieces of Tygon tubing to the condenser. The tubing to the lower connection goes to the water source, the upper connection goes to the drain. Remember, in through the bottom, out through the top. If you are using a steam bath, connect it to two pieces of Tygon tubing: one to the lower and one to the upper connection. The tubing at the upper connection goes to the steam source, the lower one goes to the drain. Make sure all of the glass and tubing joints are tight before turning on the cooling water and the steam. Begin heating the round-bottom flask carefull y.