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Author: Subject: Steam distilation question
Jackson
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[*] posted on 28-11-2018 at 10:17
Steam distilation question


Hi, I dont currently have a distilation setup but I do have a boiling flask and a relatively high tempature tube that fits into it. I want to do some steam distilation of orange and lemon peels to get the limonene. Could I stick the tube into the top of the flask with orange peels and water in it and then put the end of the tube into a container of water or should I wait until I can get a real distilation setup?
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Tsjerk
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[*] posted on 28-11-2018 at 10:22


Wait, you will get suckback problems.
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Jackson
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[*] posted on 28-11-2018 at 10:36


Will i get suckback problems if I remove the tube from the water after it is done distilling and before it cools down?
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Sulaiman
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[*] posted on 28-11-2018 at 10:49


As long as you are boiling water / making steam / creating bubbles,
you will not get suckback.

What might happen if a (waxy) substance blocks the tubing ?




CAUTION : Hobby Chemist, not Professional or even Amateur
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Tsjerk
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[*] posted on 28-11-2018 at 11:24


Quote: Originally posted by Sulaiman  
As long as you are boiling water / making steam / creating bubbles,
you will not get suckback


As long as, but how are you going to react in less than seconds upon the moments it boils a bit less?
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Polak Chem!
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[*] posted on 5-1-2019 at 09:27


Patience!
I would invest in a cheap distilling setup.

There are some really cheap ones on ebay :)
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[*] posted on 5-1-2019 at 10:59


https://www.ebay.com/itm/Vacuum-Distillation-Apparatus-24-40...
33 bucks free shipping full distillation set. They also sell 1000ml and 2000ml and 24/40 distillation setups.
Pretty cheap investment for what you get out of it.
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Swinfi2
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[*] posted on 6-1-2019 at 01:03


If you have enough pieces you can cobble together something like this:

20181010_203632.jpg - 918kB

Inspired by one of nurdrage's videos.

From what you said i think your best option is (like i have here) a siphon return to the boiling flask and i can leave it (without refilling every 20 mins) for the 3 or so hours a steam distillation takes.
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Ubya
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[*] posted on 6-1-2019 at 07:55


Quote: Originally posted by Swinfi2  
If you have enough pieces you can cobble together something like this:



Inspired by one of nurdrage's videos.

From what you said i think your best option is (like i have here) a siphon return to the boiling flask and i can leave it (without refilling every 20 mins) for the 3 or so hours a steam distillation takes.

the part of the message where he tells that he doesn't have a distillation kit, just a boiling flask and a tube should be enough to understand that your setup can't be done





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S.C. Wack
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[*] posted on 6-1-2019 at 10:26


No glass or video is necessary for steam distillation...the greatest need is an effective system that doesn't waste your time and materials. As usual the OP tries to get around what is really needed, in this case a condenser, which can be just PVC with caps epoxied to copper tube and a couple holes drilled in for water. A ground glass version will not perform better, get real steam from a steam generator for that.

A tube extending from the bottom of one's steam generator to above it may do wonders for pressure issues.




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lordcookies24
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[*] posted on 6-1-2019 at 14:56


i would say invest in a distillation apparatus is worth it.
https://www.amazon.com/NANSHIN-Glassware-glassware-Distillat...
you can buy one for around $30




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happyfooddance
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[*] posted on 6-1-2019 at 15:48


If you are looking at steam distillation to extract a small amount of limonene (5-10ml), you will need a flask or apparatus that can accommodate more than 2L of plant matter. So basically a 5L flask.

If you are looking for a more reasonable amount (say, 50ml), you'd better start looking outside of glass, because you are not going to find glassware that size (20L+) for cheap.

Also, if you are trying to really get limonene for the limonene, I wouldn't do it by steam distillation (though I have done it before), because it is not efficient and is certainly not extracted this way commercially (despite what you may have read somewhere). I would extract it with a solvent (since I don't have equipment to mechanically extract it, atm), dry over sodium sulfate, remove solvent, distill under vacuum.

This can be done for under $200.

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[*] posted on 6-1-2019 at 16:46


Quote: Originally posted by happyfooddance  
If you are looking at steam distillation to extract a small amount of limonene (5-10ml), you will need a flask or apparatus that can accommodate more than 2L of plant matter. So basically a 5L flask.

If you are looking for a more reasonable amount (say, 50ml), you'd better start looking outside of glass, because you are not going to find glassware that size (20L+) for cheap.

Also, if you are trying to really get limonene for the limonene, I wouldn't do it by steam distillation (though I have done it before), because it is not efficient and is certainly not extracted this way commercially (despite what you may have read somewhere). I would extract it with a solvent (since I don't have equipment to mechanically extract it, atm), dry over sodium sulfate, remove solvent, distill under vacuum.

This can be done for under $200.



i used a 1L erlenmeyer flask half full of peels (filled more i would get overflow in the condenser) and i got 5-6ml from a batch, if you use 1L round bottom flask there's more surface for bubbles to escape so a 1L flask is ore than enough for small batches. i did 3 batches in 2 hours, the limonene distills pretty much all at the beginning, i would distill 200ml of water (containing about 5ml of lemonene), clean the flask, separate the limonene from the oil with a separatory funnel and repeat. if you can't go big just do more batches, there's no need to buy a 5L flask to distill some limonene for fun





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