02-23-04 12:23
No 490572
Hi there!
I set up a steam destillation with an external steam-source. I put the plant material where it has to belong to (a 1 litre 3-neck-flask half full with plantmaterial) and put the hose in the plant material. started up the heat and let it destill.
BTW the place the destillation setup stands hasnt got a faucet, so its impossible for me to cool the Liebig-condenser, but I attached a second recieving flask with a rubber-hose which has caught the steam from the vakuum-outlet
Is it normal that I get about 1 litre of destillation when i let it process for about 3 hours?
Is it normal that the destill is a bit oily (in fact i dont see any oil-drops) but too much aqueous?
Is it normal, when I salt the destill out that NO LAYERS FORM??
I am very depressed..... please help me... What did I do wrong?
- Do I need to cool the Liebig?
- More steam?
- More plant material?
- More intelligenz?
Es werden mehr Menschen durch Übung tüchtig als durch ihre Ursprüngliche Anlage. -Demokrit
(Guardian)
02-23-04 13:05
No 490578
BTW the place the destillation setup stands hasnt got a faucet, so its impossible for me to cool the Liebig-condenser
That is simply not true, there are a few methods for cooling condensers without a faucet, that are easily found in the search engine.
regards,
m_e
Unipolar Mania, It's good for life...
(Newbee)
02-23-04 16:29
No 490598
So, I fucked up my entire destill because the heat burned the alkaloid?
I ask me, if it where suitable to heat the steam, additionally
Es werden mehr Menschen durch Übung tüchtig als durch ihre Ursprüngliche Anlage. -Demokrit
(Newbee)
02-23-04 23:14
No 490658
A $13 fish tank water circulation pump immersed in a 5 gal. bucket containing ice water is the easiest way I can think of to cool a condenser w/o access to a faucet. Connect the hose from the pump to the water inlet on the condenser w/ rubber tubing and run the outlet hose back into the bucket.
(Newbee)
02-24-04 05:56
No 490743
So...
I have asked so many questions, i bothered nearly everybody of you, but...
...everytime I asked my questions, everytime I got the answers. Thanks!!
And if I have to ask only ONE further question before I die, I would ask this one:
"Will DalaiLhama have success on the destillation, when he uses overheated steam AND cooling the condenser? With "success" i mean that the alkaloid will drop down in the recieving flask like "oil" - just like the way it has to be?"
Es werden mehr Menschen durch Übung tüchtig als durch ihre Ursprüngliche Anlage. -Demokrit
(Hive Bee)
02-24-04 07:39
No 490752
Gringo are you just using dry raw plant in your flask? If so, you will burn the plant and get nothing. Secondly, alkaloids are naturally present as polyhydrates of weak acids (or something like that..) and as such, steam will not liberate them, and they get 'trapped' in the plant fibres. You need to add alot of NaOH solution to make the alkaloids freebases, so that when the steam is bubbled through, it will grab the fb-goodies; and u will have a lot more fun.
Also what plant are u using because some plant alkaloids will be visible as a separate oily layer, others (eg freebase pseduo, eph etc from ephedra) are not. I repeat, you will not have a big fat oil layer when distilling ephedra alkaloids (you may see a few light droplets at the most). That said, they are still present and a spaced out throughout the entire distillate (so u cant just remove the top layer to isolate). Meth freebase on the other hand, is nice and fat and imiscible with water.
And yes, 1) superheating the steam and 2) heating the flask contents to near boiling (~95`C) and 3) cool water circulated through your condenser are almost essential to success.
(Newbee)
02-24-04 09:59
No 490763
But can you remove this question, too. please...
What do you mean with "just remove the top layer to isolate"?
Arent there enough alkaloids to form layers, or why is ephedra so... wierd?
Es werden mehr Menschen durch Übung tüchtig als durch ihre Ursprüngliche Anlage. -Demokrit
(Hive Bee)
02-25-04 00:16
No 490885
What do you mean with "just remove the top layer to isolate"?
Arent there enough alkaloids to form layers, or why is ephedra so... wierd?
Some if not MOST of the freebase ephedra alkaloids are PARTIALLY soluble in water, and as such, do not float on the top of the water distillate (like meth does). For this reason, they cannot be isolated by removing the 'top' layer or portion of the distillate. (as they are dispersed throughout the ENTIRE distillate)
SO BASICALLY, u need to pH and evap the whole lot (easiest). Or absorb the freebases into a NP then titrate or gas (hardest).
(Newbee)
02-26-04 11:55
No 491207
That sounds like the right motivation...
To absorb the freebase in NP, you simple dilute the NP in the destilate? Shake a bit and seperate? gas the separated and "heureka": Ephedrine-HCL?
BTW: WHY are the alkaloids partially soluble in water?
Es werden mehr Menschen durch Übung tüchtig als durch ihre Ursprüngliche Anlage. -Demokrit
(Hive Bee)
02-26-04 14:03
No 491223
To absorb the freebase in NP, you simple dilute the NP in the destilate? Shake a bit and seperate? gas the separated and "heureka": Ephedrine-HCL?
Yeah thats right. 3 smaller pulls with the NP will be better than 1 biggy. U can combine them all together when u gas though...
BTW: WHY are the alkaloids partially soluble in water?
Because when God designed their biosynthesis and properties he made it that way... How the fuck should i know, they just are
...