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Poppy
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249 Lemons!1!!
Ok right now I have 249 lemons in my hands, freshly bushed. I'm planning to experiment with its vitamin C and citric acid.
So, any ideas, suggestions, I'll do it, it will just depend on the chemicals available to perform all the stuff here!!
Here they are, reagent grade 
[Edited on 8-13-2012 by Poppy]
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Mailinmypocket
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Grate the zest off all of them and do a huge extraction of limonene!
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cyanureeves
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lemonade for sure and maybe you can come up with some kind of mosquito repellant. mosquitos hate lemon grass so maybe they dont like lemons either.
[Edited on 13-8-2012 by cyanureeves]
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Poppy
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Mailinmypocket:
Lemonene theorically is said to be distillable without decomposing. But the ammounts that would be found are so small a solvent extraction must be
performed in place. Guess alcohol will do it? Familiar to limoncello liquors?
After peeling..'n smashin... Yuurayy! Lemonade for half a year! As they would never survive invitro like that, instead let they feed the backyard
chem! Look, Im not torturing the lemons, they would rotten anyways!
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Mailinmypocket
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Steam distillation of the zest goes quite well, although I should have said orange/lemon oil and perhaps not limonene specifically. I can't find the
procedure I followed a few months back when I steam distilled orange oil, below is a similar process except I extracted the oily layer from the
distillate with ether and dried that over sodium sulfate and distilled off the ether which gave a powerful smelling extract reminiscent of the scent
of Pledge furniture cleaner.
http://www.rsc.org/learn-chemistry/content/filerepository/CM...
Upon further searching I found this more in-depth experiment on extractions:
http://infohost.nmt.edu/~jaltig/SteamDistill.pdf
I thought it was more interesting to isolate the product as much as possible using a solvent extraction of the distillate
[Edited on 13-8-2012 by Mailinmypocket]
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hyfalcon
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D-limonene is a byproduct of making orange juice. I don't think it even takes steam to get the orange oil out of the peels, they just press it. The
d-limonene is a fraction of the expressed orange oil, about 85-90% I think if I remember correctly.
[Edited on 13-8-2012 by hyfalcon]
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Poppy
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85%???
Its seems reliably easy to do the extraction. For it will render the first usage of my distillation apparatus!!
Later on the oil will be kept and, after producing ether, further extracted according to the files you provided above.
It's a lot o peel, hope it works, I just have to improvise hooks for my glassware
Thx
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Nicodem
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Thread Moved
13-8-2012 at 06:51 |
vmelkon
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I say do it.
I did it a couple of weeks ago using orange peel. I had been collecting the peels for months every time I eat an orange and I put it in the freezer.
The stuff that distills over is mostly water and a tiny bit of limonene. The limonene floats on top of the water. Once finished, I left the bottle on
a table but after a while, it a film formed on top of the limonene. I placed the bottle in a freezer for now.
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Poppy
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Here they are! Ready to bake!
Obs.: Did you pickled the peels in small chips? Once you finish the distillation they would never come off the mouth of the baloon the way they are !
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Mailinmypocket
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Quote: Originally posted by Poppy  | Here they are! Ready to bake!
Obs.: Did you pickled the peels in small chips? Once you finish the distillation they would never come off the mouth of the baloon the way they are !
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Nice! You will have a much larger batch than I did As for the skins I used a
cheese grater to scrape the colored part of the skin off and then used a blender to pulverize it even further into a mash which looked like a bright
orange stew in the rbf as seen in the first picture
The second picture is what the distillate looks like, you can see small droplets of oil sticking to the glass
The third picture is the yield from 5 large oranges after a DCM extraction of the distillate
  
*edit* Why are you baking the peels? Is it to preserve them for doing the extraction later on?
(sorry for the second picture being sideways, it's the only way the forum let me upload it)
[Edited on 13-8-2012 by Mailinmypocket]
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Poppy
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| Quote: Originally posted by Mailinmypocket |
As for the skins I used a cheese grater to scrape the colored part of the skin off and then used a blender to pulverize it even further
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What? Did you scraped it directly from the fruit? It seems hard to pick the peels individually
No no.. noo! Haha its use of the habit I mean't "Baking" as referring to processing all this stuff.
EDIT: Between, my condesator is a Grahan Type, 600mm long. Guess the oil won't get stuck there, at least not if I process the whole of the peels?
[Edited on 8-13-2012 by Poppy]
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Mailinmypocket
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Ah! Of course, baking! lol
Just run the distillation for a bit after the distillate is no longer milky looking which indicates no more oil is coming over... The steam and water
should flush out the residues that are in your condenser.
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dennisfrancisblewettiii
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Lemon pie. Lemon meringue pie. Lemon sherbert. Lemonade... mmm
[Edited on 14-8-2012 by Genecks]
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Poppy
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Alright I have now synthesized, from the aproximately yield of 12L of juice, more than 500g calcium citrate.
Mold is so cruel,it would consume all of the lemon contents in a matter of days, extracting the citrate was a priority!
Calcium citrate is a very low density substance, it forms upon heating lemon juice in a stainless pan to no less than 70 degrees celsius, and then
throwing a 10% stoichometric excess slurry of calcium hydroxide and boiling water into it, filtering the content with a household strainer, and
drying. Oil strainer suits best. Calcium citrate can be put to dry in the oven or open air.
The peels are two days old now. Hopefully the oil has not deteriorated. Tomorrow the distillation shall be carried out as by now I was privated of
the proper supports for the apparattus, which were now provided.
If anyone's interested I'll post a picture on the citrate later on.
Ah! and Grandma Saint Edwigs must certanly have dilicious recipes profiting from the usage of citric acid!!!
[Edited on 8-15-2012 by Poppy]
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vmelkon
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| Quote: Originally posted by Mailinmypocket | Ah! Of course, baking! lol
Just run the distillation for a bit after the distillate is no longer milky looking which indicates no more oil is coming over... The steam and water
should flush out the residues that are in your condenser. |
Once I was finished with my oranges, I cleaned my 1 L flask, then added some water and distilled. It helps to clean the insides of the glassware
(condenser, claisen adapter, glass stoppers, thermometer sidearm adapter).
[Edited on 15-8-2012 by vmelkon]
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Ephesian
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| Quote: |
Ok right now I have 249 lemons in my hands
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Wow you must have very large hands 
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Poppy
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OMGosh, blame on my parents. They threw away my lemon skins, in fact I took them out of the freezer to melt its ice, but forgot it for too long and in
a matter of a single day it rottened 
Below a pitcure of my distilling apparattus. A lot of trouble occurred with this, causing delays that untimately led to lemon skin failure.
For some reason the amianthus plate diminishes much the heating power of the flame to the point water drips veeery slowly from the tip of the
condenser.
[Edited on 9-2-2012 by Poppy]
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Poppy
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double post
[Edited on 9-2-2012 by Poppy]
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vmelkon
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Is that a 3 L flask? I like the graham condenser. That is very long. As for the receiving beaker, I would use something that has a lower diameter to
help the droplets of limonene coalesce. Remember that a lot of the distillate will be water and there will be very little limonene floating on the
water. Some of the limonene will stick to the sides of the beaker and won't even rise to the top of the water.
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Poppy
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vmelkon,
That's a 1L flask. The two liters one, bigger, cracked on stading directly upon flame.
There must be a heating process which works best, like oil bath, sand bath or even copper powder bath someone has mentioned around. Guess there can be
made a "poorman's" iron powder bath LOL
Whatever, distilling like that is unbelievebly crazy and some kind of solvent extraction must come in place.
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Mailinmypocket
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Try using a hot plate and making an air bath to heat the flask, you can make a tin foil tent around it to keep the heat in. Also, I would suggest
getting one of these U adapters... It would allow you to run your graham condenser vertically. As it is, it won't perform perfectly since the
condenser is at an angle. It creates these "traps" of condensate which make it hard to have a good flow of vapor.
Check here for the adapter mentioned!
Solvent extraction of citrus, in my experience, is annoying and difficult.. The result is always colored with fruit pigments and you need to mash it a
lot and let it soak in the solvent. Then getting the citrus oil out of that is hard because you need to distill the solvent out to get a concentrate.
The concentrate becomes this gunky stuff which is hard to clean, let alone get the oils out of.
Your set up looks good actually, all you need is one of those U adapters to properly attach the graham.
And also, grate the skins off the lemon with a fine grater. Its a pain in the ass but just shave the yellow off the lemons and then blend the skins in
a blender into a paste. Add the paste to water and boil that in your distilling flask! I've always has great results
[Edited on 2-9-2012 by Mailinmypocket]
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S.C. Wack
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Google: ecuelle a piquer
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Poppy
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Alright seems the adptor is really needed indeed. Sometimes the condenser spills the loaded water like puke, its not anything even close to a
constant flow.
As for the process Écuelle à Piquer, what a hell is this? How exactly it works?? Google says it requires a high speed motor and also one must
elaborate the proper spikes, I think its promissing if ammounts like those 249 lemons are loaded each time.
Mainlimypocket, as you showed, the yield is quite high really, destillation may work fine.
As for solvent extraction, If suitable alcohol is used, you can soak that for a couple days, filter the zest, recycle the alcohol 5 or 10 more times,
then bring the alcohol to oxydise with dichromate, this will make the alcohol evaporate as gaseous aldehyde, while the dichromate wont hurt the
lemonene, since its just like a horned aromatic. What about it?
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Lambda-Eyde
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| Quote: Originally posted by Mailinmypocket | Also, I would suggest getting one of these U adapters... It would allow you to run your graham condenser vertically. As it is, it won't perform
perfectly since the condenser is at an angle. It creates these "traps" of condensate which make it hard to have a good flow of vapor.
Check here for the adapter mentioned!
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Reading this reminds me of how pissed off I am at those cocks on eBay selling distillation kits with graham condensers mounted horizontally. Why the
hell are they specializing in selling something they don't even know how to use?
[Edited on 2-9-2012 by Lambda-Eyde]
This just in: 95,5 % of the world population lives outside the USA
Please drop by our IRC channel: #sciencemadness @ irc.efnet.org
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Mailinmypocket
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| Quote: Originally posted by Lambda-Eyde | | Quote: Originally posted by Mailinmypocket | Also, I would suggest getting one of these U adapters... It would allow you to run your graham condenser vertically. As it is, it won't perform
perfectly since the condenser is at an angle. It creates these "traps" of condensate which make it hard to have a good flow of vapor.
Check here for the adapter mentioned!
|
Reading this reminds me of how pissed off I am at those cocks on eBay selling distillation kits with graham condensers mounted horizontally. Why the
hell are they specializing in selling something they don't even know how to use?
[Edited on 2-9-2012 by Lambda-Eyde] |
So stupid! They just try to mount something that looks as sciencey as possible. In this configuration a liebig would probably be the way to go.
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