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Brightthermite
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[*] posted on 6-8-2020 at 09:51
Distillation Ideas


I recently purchased a fractional distillation set up. It was purchased to purify and concentrate some sulfuric acid I have, but before I try that I would like to become familiar with the set up and distillation. Any suggestions on useful and easy things to distill starting out while I get the hang of it?
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Fyndium
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[*] posted on 6-8-2020 at 10:14


Acetone, ethanol, toluene, anything you may need. I routinely recycle solvents by collecting them in separate bins and then distilling them pure in boring days.
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BromicAcid
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[*] posted on 6-8-2020 at 13:05


Water, just water. Nothing flammable, nothing corrosive, just boring old water. Check the height of your head thermometer, make sure you read 100°C. If you've got a packed column see what it takes to flood it, not flood it. You better have some stirring because sulfuric bumps like crazy, so check out the effect of stirring. Really get the hang of it. If you've got vacuum apply it, stop it, rinse and repeat. No sense messing with anything potentially dangerous, just have fun with it. Count drips to determine the takeoff, increase and decrease temperatures. Take readings as if it were your job.



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TLutman
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[*] posted on 6-8-2020 at 14:20


I’m curious what substance has a bp close enough to sulfuric acid to necessitate fractional distillation? I would worry about cracking glass with the inevitable bumping, and I had issues with water flashing to steam, sending a huge vapor cloud that cleaned out the condenser several times. I would think with the energy needed to reach the top of a column, you will experience similar
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fdnjj6
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[*] posted on 6-8-2020 at 14:28


I tested my setup using a steam distillation of limonene. Nothing crazy. Especially using it for the first time you need to make sure everything works and you don't want to end up like the guy I just read about on here who's brand new flask just decided to break for no reason even though he was doing every single thing correctly and not abusing his glassware.

Once the water/steam distillation is done, move on to distilling things like ethanol and other useful solvents. Don't distill ether though. It's too much of a fire/explosion hazard and many have been killed doing so. So stick to relatively tame stuff. I would discourage nitric acid distillation until you really have things down and know what baths to use.
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B(a)P
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[*] posted on 7-8-2020 at 02:39


Plus one to what @BromicAcid said. It removes all variables and the hazards so you can focus on the process and the performance of your equipment..
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Brightthermite
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[*] posted on 7-8-2020 at 10:26


Thanks for the ideas. I am going to start with water as was suggested, once I practice and feel confident I will try a solvent. Besides distilled water is useful :D
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[*] posted on 7-8-2020 at 12:00


Put some food colouring or similar in your cooling water. In the event of spills or leaks it helps work out what is going on/what has gone where.
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[*] posted on 18-4-2021 at 18:03


Quote: Originally posted by Brightthermite  
Thanks for the ideas. I am going to start with water as was suggested, once I practice and feel confident I will try a solvent. Besides distilled water is useful :D


be careful, if you distil 2 or 3 times tap water your flask get a white layer of fluorine or another shit and never get cristal clear again...

I "ruined" a expensive 10L reactor distilling tap water. now the glass have "cataracts". I read in a place a guy putting fluorine + nitric acids to return to cristall clear but I lost this data or where I read it? wow too much surfing! :-)
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zed
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[*] posted on 18-4-2021 at 20:13


Most likely Calcium and/or Magnesium Carbonates. Boil the flask out with vineger. Should clean it right up.
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draculic acid69
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[*] posted on 19-4-2021 at 02:39


As zed said it's mg+ Calcium carbonates. Depending on where you are tap water will vary in concentration but it's definitely carbonates of some mixture
One time I was doing the double boiler thing and little white spots start appearing on the pot and bottom of the bowl.upon tasting i found out what it was: chalk. Stuff tasted exactly like chalk.

[Edited on 19-4-2021 by draculic acid69]
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Fyndium
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[*] posted on 19-4-2021 at 04:52


I get those calcium cataracts all the time when I use water baths to heat many reactions. As the water slowly evaporates and I just add more, it concentrates the calcium and other, which are less soluble in hot water, so they crystallize onto the bath kettle and to the flask. A quick rinse with citric acid or vinegar will wipe them right off.
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[*] posted on 19-4-2021 at 06:29


obviously I rinse the flask with cheap household hcl but this only remove with fizing the carbonates in the surface ... but a bit every time, acumulative penetrate in the glass and impossible to remove, no nitric, sulfuric... piranya with 3% H2O2...

look around the mouth, cristall clear, but the body...

IMG_20210419_162540.jpg - 560kB
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[*] posted on 19-4-2021 at 06:37


Quote: Originally posted by zed  
Most likely Calcium and/or Magnesium Carbonates. Boil the flask out with vineger. Should clean it right up.


I think I make a boiling with cheap hcl and no result... but maybe try again or with nitric + hydrofluoric and if not, leave it for distil water alone.
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draculic acid69
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[*] posted on 19-4-2021 at 19:45


Quote: Originally posted by pneumatician  
obviously I rinse the flask with cheap household hcl but this only remove with fizing the carbonates in the surface ... but a bit every time, acumulative penetrate in the glass and impossible to remove, no nitric, sulfuric... piranya with 3% H2O2...

look around the mouth, cristall clear, but the body...


Maybe you got something other than just carbonates in your water.
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[*] posted on 24-4-2021 at 09:22


if not? :-)
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zed
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[*] posted on 25-4-2021 at 13:33


My local cafe owner usta clean out his Coffee pots with "Dutch Cleanser" and ice. Put a little cleanser inside the flask, with ice cubes, and swirl. The mild abrasive action may clean things right up.
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[*] posted on 6-5-2021 at 23:56


Quote: Originally posted by zed  
My local cafe owner usta clean out his Coffee pots with "Dutch Cleanser" and ice. Put a little cleanser inside the flask, with ice cubes, and swirl. The mild abrasive action may clean things right up.


this is a reactor with DN100, I can put my hand inside and the sticky shit is... well, part of the glass now? maybe with an electric polishing tool...
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[*] posted on 7-5-2021 at 00:09


Quote: Originally posted by pneumatician  

this is a reactor with DN100, I can put my hand inside and the sticky shit is... well, part of the glass now? maybe with an electric polishing tool...


Try cerium oxide.
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[*] posted on 7-5-2021 at 01:16


If it's etched, there's little you can do. Just live with it, it won't affect anything but aesthetics. After all, auctions are full of glassware that is literally covered in some sort of brown crap that is next to impossible to remove without boiling them in pure Caro's acid.

I like to keep my glassware spotless. I routinely clean them all by rinsing them with detergent and water(dishwashing soap, sodium percarbonate), scrubbing if necessary and washing everything that fits in a dishwasher. Fritted filters I clean by first washing with acetone, then using sodium hydroxide, and then citric acid, flushing with lots of water at all phases. Usually gets them shiny white, if not, I call in Mr. Piranha. In some instances I just put the glass (no frit filters, as I broke one once by this way) in oven and burn off any residues.

Fast way to dry glassware, especially frits is to rinse with acetone and let evaporate. A bit slower is to cook water off in an oven, if one is at hand.
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