Step 8: Fractionating Column

This is kind of important. There are some nasty chemicals on the surface of the copper after soldering. You probably don't want those in your distillate. Dish detergent and warm water do the trick. A long thin brush helps, the kind they make for test tubes. But whatever works. This is especially important for the tube that will become the fractionating column, since that's supposed to be pure output.

Right now your fractionating column is a lot of column and not a lot of fractionating. You need to pack it. The setup in my lab looked like it was packed with steel wool. I had my doubts about this but I went and got some coarse steel wool and tried it anyway. Don't do it. Bare steel doesn't like heat and organic compounds.

Go to the grocery store. Go down the cleaning supplies aisle. Go to the dish scrubbing section. Look for the old fashioned metal mesh dish scrubbers. There are three kinds: Stainless steel, galvanized steel, and copper. Don't get the galvanized one. Zinc is good for you in small amounts, but I don't know what the solubility of zinc is in an environment like the one you're making. Go for copper. Then you can tell your homeopathic friend that it's all copper and has healing properties and therefore you should drink this.

Remove the wire/staple that holds the scrubber together and unravel it. Kind of like a sock huh? Now get a wire/cord and feed it down your column and tie it to the end of the unraveled scrubber. Pull the scrubber though the column. Use a scissors and a needle nose pliers to trim the scrubber and pull it into position. The scrubber should reach the very bottom of the column, and stop short of the first opening of the Tee. Viola, you have a fractionating column.
<p>How much water do you think you need to flow through the condenser, and how long would a typical run be likely to take.</p><p>I am on a metered water supply so I would like to calculate how much the water is going to cost having a constant flow.</p><p>Thanks</p>
<p>Copper as a distiller is quite smart but you have to be careful with flammable materials. I could see the heat from the pan exploding with excessive pressure and flammable materials being distilled. This would be fine for fine herbs but if you are going to distill corrosive or flammable materials you need glass (pyrex).</p>
<p>Can this condenser be scaled up 2 or 3 sizes? does it even matter if its a bigger size or smaller size?</p>
<p>Can this be made entirely out of stainless steel? would stainless steel be more efficient than copper? what alloy stainless steel would you use?</p>
<p>So, if I was going to use an Erlenmeyer flask as a distillation pot, how would join the column to the flask? Any ideas? I'm a chemistry teacher with access to most glassware items but we're low budget enough to not have distillation equipment...</p>
Be extra careful to prevent pressure build up in the flask. You could try a stainless steel or copper tube inserted into a drilled rubber stopper. Use as wide a bore as possible to prevent impedance. The rubber should hold up to the temperature if you're not working with temps above 100C boiling point. Don't expect the best chemical purity since plasticizer may get into the distillate.
<p>I like the project but I bought a complete distiller condenser made from glass. Copper in my opinion would heat up to quickly and result in you getting different types of separation. It can work but copper is a good conductor of heat and electricity. Mine was a $219 dollar pyrex condenser with column distiller set up.</p>
After looking at expensive glassware ($50+) this seems very useful! I will be making one for chemistry use
<p>Instead of making the hole in the pressure cooker, you could take a rubber or cork stopper drill a hole in it to fit over the fitting coming out of the pressure cooker and then just press the pipe over the cork.</p>
Does anyone appreciate the irony that there are 12 steps in this project?
<p>didn't notice yell.</p>
<p>how do you make those diagramsof the lab equipment?</p>
<p>The images used to have captions on them with a citation. I'm not sure what happened to those. The distillation figures are from Techniques in Organic Chemistry by Mohrig, Hammond, Schatz. ISBN 978-1429219563. An excellent book worth investing in.</p>
<p>&quot;So for those of you in the non-US/UK portions of the planet, I'm sorry.&quot;</p><p>Don't feel sorry, it's not your fault! ;)</p><p>BTW: thanks for the great instructable!</p>
<p>I made mine last summer with an old aluminum pressure cooker. It works pretty well. I need to get better seals for the cooker because there is a good amount of losses. the way I joined the copper fitting to the lid of the cooker was by drilling out a hole and tapping it with pipe thread and joining it with a fitting. It worked really well.</p>
<p>Hey, that looks great! I had to do a double take because it looks so much like mine. Nice work, and I'll keep the tapped hole idea around for the next project. </p>
web site http://homedistiller.org/forum/viewtopic.php?f=3&amp;t=5041
is this good enough or should i keep going i found these sights in 5 min do your research before you brew 'PLEASE'
sorry you can do it if you want to i will not make my spirits in it and personally wouldn't drink it but go ahead not trying to sound rude it just isn't for me
I just don't want anyone to 'DIE'
I understand your concern but I disagree. From a scientific standpoint I wouldn't exactly call answerbag.com or yahoo answers references. There is one linked paper from India that looks reasonably legitimate which states, <br> <br>&quot;Therefore, it can be suggested that general neurotoxicity produced by aluminum is not modified by ethanol. However, the aluminum load caused by aluminum exposure, may be influenced by ethanol co-exposure.&quot; <br> <br>In other words, ethanol MAY help your body absorb more aluminum, but doesn't convert aluminum into poison. The same could be said of having a beer with the meal you cooked in an aluminum pot. <br> <br>The methodology of the paper included dissolving large amounts of aluminum in &quot;nitric acid, sulphuric acid and perchloric acid in the ratio of 6:1:1&quot; and feeding it to rats. Wort is slightly acidic, nowhere near H2SO4 and HNO3. <br> <br>Aluminum metal is highly reactive. It reacts with oxygen to form Al2O3, which is one of the most stable compounds known. It's sapphire. It's sandpaper. Any aluminum exposed to air will immediately form a coating of Al2O3. Al2O3 has a boiling point of 2,977&deg;C, which is a little hotter than a pot still can get. Other aluminum compounds tend to have extremely high boiling points or undergo decomposition at high temperatures before being able to boil. That means aluminum in a pot still is very unlikely to make it out of the pot still, since that requires the aluminum compounds to boil. <br> <br>You might run into a few more problems if the condenser was made of aluminum. Or if the container used to store the spirit was made of aluminum. But I very much doubt an aluminum pot still could do anything worse than if your grandmother cooked you some spaghetti sauce in an aluminum pot. <br> <br>I understand the &quot;better safe than sorry&quot; mentality. Aluminum is kind of a touchy topic. There is a lot of pseudoscience surrounding relatively mundane things like aluminum, copper, magnets, vaccines, etc. But there is a big difference between informed caution and fear mongering. Given the evidence considered here I hardly think warnings of death are warranted.
DO NOT EVER USE aluminum to distill spirits you will poison your self or someone else aluminum poisons spirits use copper or stainless PLEASE
That's an important claim if it's true. I haven't found any good documentation of that. Can you please provide a reference?
I like the way this instructable is laid out, very easy to follow. I have heard that crushed glass works great as copper pot scrubbers are somewhat hard to find. If accessible, well sanitized auto glass breaks into nice small pieces, just right for this application.
To be certain that you get the most efficient flow of coolant and also more surface area inside the condenser, could one step up the dia. of the tubes used for the condenser chamber? Say inner tube 3/4&quot; and outer at 1.25 or 1.5&quot; even? <br>
thank you <br> good post clears up my problem.
Hello sir <br> I understand most of your design but am having trouble with the thermometer. were is the sensor located.is it in the column above the packing. I'm just not sure.
The sensor (thermocouple) is the silver probe which is stuck all the way through the rubber stopper at the very top of the vertical column. You can use a regular thermometer if you wish, but digital thermocouples are not hard to come by, and they are much more accurate. Just be sure to get one that has a rigid metal probe. This one or anything similar would work: <br> <br>http://www.ebay.com/itm/LCD-Type-K-Digital-Thermometer-TM-902C-2-Thermocouple-Probe-/190579208001?pt=LH_DefaultDomain_0&amp;hash=item2c5f67ef41 <br> <br>The probe should be positioned to read the temperature of the vapor right where the vapor travels through the T section on its way to the condenser. Don't let the probe touch the column packing or the side of the column, and be sure the probe is sticking through the stopper, not with the tip inside the rubber. It should be measuring the vapor temperature only.
Vaary nicshe, a'll drink to thish, hic
Hi<br><br>Nice looking fractional pot still, I would have tried to find 304 or 316 stainless for it because of the pain in the ass cleaning of copper after each run or you get opper sulphate in it and then you go blind, but keep the copper scrubbers because if theres no copper at all there will be an unpleasant rotten egg smell<br><br>Looks like your running it a bit to fast, to get a purer spirit it should be about 80 deg c - for a pot still might be a bit higher but not to close to 100c<br><br>Nice job in the soldering make sure it's lead free solder or you will get led poisoning without a gun involved hahahaha but seriously it's no laugthing matter <br><br>Heres my setup<br>All glassware and fits to a modified 50 litre keg<br>
http://www.labdepotinc.com/Product_Details~id~761~pid~59709.aspx <br> <br> <br>I found this from a chemestry supply store for $250... do you mean that glasss would be safer to use... and are you saying coppy plays a role in filtration? <br> <br> <br>
Thank you for this tip: <br>&quot;If you want a clean-looking joint (no solder blobs), quickly (before the solder solidifies) brush the exterior of the joint with the flux brush AWAY FROM YOUR FACE. This will remove the majority of the exterior solder drippage.&quot; <br> <br>I'll try it next time I plumb, for whatever reason!
This pressure fitting is gas tight? Does the lid just jam tight against the edges of the copper female adapter?
Sorry for the slow reply. There is a very small amount of leakage when using the fractionating column, about as much as what escapes from the emergency pressure release thingy (to use the technical term). I may seal this with epoxy at some point but it hasn't been a big problem so far.
A very old school way of sealing small gaps in a still was to mix a dough of just flour and water and use the paste to seal any small holes- the advantage to this is that it is non-toxic- when you are done wash it of and reapply next time- no risk of hot liquids/ gasses/ being affecting the epoxy or the epoxy contaminating your process.
Actually I tried this method. I must not have done it right because it didn't work very well. I was probably supposed to let it dry. I get a little frantic and impatient at the end of a project. I'll have to try it again next time.
A BIG Thank You to everyone who voted for me in the Mad Scientist Fair! You guys rock!!
Here's my setup.&nbsp; It's almost identical to yours, except for a few modifications. My coolant is a closed loop using an aquarium pump I had from an old computer water-cooling setup.&nbsp; I found some great 3-way fittings at Home Depot that were like 1/2&quot; - 3/4&quot; reducing couplings but with a 1/2&quot; fitting coming off one side. I drilled out the retaining lip inside, put the fittings on either end of the 3/4&quot; tube, then passed the 1/2&quot; tube through it.&nbsp; soldering was interesting, but not terribly difficult.&nbsp; I also forewent the screw fittings to save a bit on cost, and just slip-fit the pieces.&nbsp; I was able to tap 3/8 NPT threads into the pressure relief valve without even affecting the valve seat, so I can even still use it as a pressure cooker.&nbsp; Let me know if you see something you're curious about.
I thought about trying to use the threads that were already in the cooker. I'll have to try that out next time I make one of these.
I am sorry aeturnusjunk but a metal still is not &quot;laboratory quality&quot;. Glass is used in laboratory stills to minimise metal ion contamination. Also hot copper is sufficient to catalyse reactions with ethanol.<br> <br> <a href="http://www.sciencemadness.org/talk/viewthread.php?tid=8709">http://www.sciencemadness.org/talk/viewthread.php?tid=8709</a><br> <br> People do get away with copper stills all the time by avoiding hotspots, even commercially, but it is risky.
Sorry, I didn't mean to discourage you. You don't have to be a glass blower though, in the lab we use QuickFit glassware<br> <a href="http://en.wikipedia.org/wiki/Quickfit_apparatus">http://en.wikipedia.org/wiki/Quickfit_apparatus</a><br> - expensive but very good and lasts. Before quickfit we used to use glass tubing and corks.<br> In industry potable liquids including wine, beer and spirits are processed through stainless steel. When I was a teenager I made a water purification still from aluminium. The tank eventually corroded but it provided many years of service.&nbsp;<br>
In the alcohol industry they use copper because during fermentation the yeast puts out sulfides. Using copper will remove these from your distillates as it works.<br><br>At least that is what I have been lead to believe.
Yes some commercial stills like the Coffey Patent still are made from copper and often hillbilly stills had a copper cooling coil. But these stills are not Lab quality; the small traces of copper ions introduced would be unacceptable. Keep in mind that the most significant use of stills in the lab is for the production of highly purity distilled water.<br>When copper is used in alcoholic beverage industrial stills care is taken to ensure that no hot spots occur that could cause the reduction of alcohol to aldehyde. The small trace of copper introduced into alcohol during contact at low temperature is usually low enough that drinkers are not at much risk. <br>Yeast doesn't produce significant sulfides during fermentation, though often H2S is used to destroy wild yeasts in the ingredients before the introduction of the yeast culture. Sulfides are pretty toxic to yeasts. The low pH of the must would make the formation of copper / sulphide compounds unlikely, most trace sulfides end up as gaseous H2S and leave the system.
Yeah! The quickfit is the type that inspired this project. When I'm rich I'm definitely going to invest. Pricing is a little steep, but actually not as bad as I thought. The condenser goes for $67US on Aldrich.
Dang. You got me :) As soon as I learn how to blow lab glass I promise to redo the instructable. This still probably won't be getting hot enough to significantly catalyze ethanol in that particular way, but it's true that this project is far from laboratory quality. *sigh* A man can dream. I modified the name, so as not to trouble my fellow science-types. Nice catch, thanks for letting me know about this one.
http://www.leeners.com/ <br>^they sell malt, yeast, and pretty much everything needed to brew your own beer/wine (or illegal liquor)<br>

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Bio: I'm a graduate student in the Materials Science department of the University of California at Santa Barbara. I made these Instructables while I was ... More »
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