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DrugPhreak
Working Bee
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| Joined: 07 Mar 2005 |
| Posts: 114 |
| Location: Bee Hive |
4261.30 Points
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Extracting 8% Ephedra
Sun Jul 03, 2005 8:36 am |
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| SWIDP has obtained a decent amount of 8% Ephedra and is looking for the best write-up for extracting it. SWIDP searched on this forum and the offline Hive archive and found nothing, but there was a link to a post on the online Hive archive, which is of course inaccessible at the present time so it could not bee read. If someone has a good write-up for this please post it. |
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2spun
The Resistor
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| Joined: 17 Feb 2005 |
| Posts: 172 |
| Location: daMaGe'd |
3344.98 Points
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re: Extracting 8% Ephedra
Sun Jul 03, 2005 12:54 pm |
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im not sure that would help swidp, as i think what hes talking about is the standerdized crude alcholic extract of ephedra.
in which case hed probobly want to do an a/b extraction, make sure to use plenty of base (to turn the polyphenols into phenolates which stay in water) and salt as it has a habit ofmaking emulsions. |
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DrugPhreak
Working Bee
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| Joined: 07 Mar 2005 |
| Posts: 114 |
| Location: Bee Hive |
4261.30 Points
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re: Extracting 8% Ephedra
Sun Jul 03, 2005 9:25 pm |
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Ummm... a Soxhlet might be of use. Yep, this is the 8% standardized Ephedra Sinica. SWIDP has never been able to get this before, but they have extracted alkaloids from non-standardized Epedra Sinica many times, but that's a buttload of work for very little return. So just an A/B then? Do you think a sand filter would be necessary when working 8% also etc? SWIDP plans to extract this pretty much the same way they extract Mimosa Hostilis, but adding base first of course. This 8% Ephedra seems to be standardized mainly with PSE so SWIDP was also thinking about steam distilling, but they probably won't do that. Does anyone that has extracted 8% Ephedra have some crucial advice for SWIDP? |
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dwarfer
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| Joined: 24 Apr 2005 |
| Posts: 4 |
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142.44 Points
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re: Extracting 8% Ephedra
Tue Jul 12, 2005 4:10 am |
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Presuminhg this is powder?
Place in pressure cooker with 2X alcohol. Heat to 90C, cool, decant alcohol.
Do this twice. Use cheapo $8/gal mixed alcohols.
Combine decantations.
Filter the alcohol thru a MCC buchner-type filter set up.
(sand trap but using pool filter microcrystalline cellulose)
========
Fling the top scrapings off your Buchner back into the now-dry pressure cooker.
Hope it's not aluminum, but SS:
cause now you are going to base the hell out of it with strong NaOH:
and Al's amphoteric nature won't like it , much..
Heat to near boiling, cover with Xylene.
Using your handy drill-mounted blender-stirring device,
beat the crap out of it. Decant the xylene after it settles.
Throw some NaCl into the warm goo, and repeat with the xylene.
Filter the xylene.
Add the xylene and the alcohol extracts together.
Heat the blend while stirring to 90C. If particulates form on the way up
the temperature scale, re-filter and keep going.
By 90C all alcohol should be gone.
Cool.
Gas.
viola.
guaranteed 90% +, or your money cheerfully refunded.
( Doubt if you will get 8% though..
they lie....)  |
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loki
guinea pig
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| Joined: 09 Mar 2005 |
| Posts: 391 |
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14167.88 Points
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re: Extracting 8% Ephedra
Tue Jul 12, 2005 5:57 am |
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Wouldn't a boil with chalk work better for eliminating pesky acidic polyphenols?
Did a failed experiment with another species of plant and seemed to have been most confounded of all by sugars. (damn bitches seemed to hang onto my goodies !)
Having now witnessed the magick of the STB III, like every new thing i get my hands on i want to know if it works for other things... Seems to me that the combination of citric acid and salt together would interfere with sugars and tannins just as it interferes with synthetic polymers, citric steals the space for sugars (being a sugar derivative itself) and the salt ensures that upon filtration only things of ionic nature more soluble than sodium chloride (ie many common alkaloids, especially the one in question). Extracting to the freebase, imho, is what you always do unless you can't, cos it's usually more quick and produces prettier crystals. Precipitating naptha extracts directly is lots of fun, although i think probably it's better to overdo naptha and then gently reduce it until it saturates, so one can do things like drying it and washing it.
Exploiting the selective solubility of salts of the primary and perhaps secondary alkaloid in the process would probably help ensure it's not just x50 that you end up with, and something that you desire to steal oxygens or hydrogens from (just a personal preference against non-methylated alphamethyl phenethylamines). Doing this separation requires oxalic acid as the distinct isomers have opposite behaviors in alcohols and water. |
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DrugPhreak
Working Bee
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| Joined: 07 Mar 2005 |
| Posts: 114 |
| Location: Bee Hive |
4261.30 Points
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re: Extracting 8% Ephedra
Thu Jul 14, 2005 12:52 am |
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| Thanks for the info... this may come in handy. SWIDP would be happy if they just got 10gm of this non-gakked feed for a nano. |
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Elementary
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| Joined: 18 Apr 2005 |
| Posts: 100 |
| Location: UK |
3449.86 Points
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DrugPhreak
Working Bee
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| Joined: 07 Mar 2005 |
| Posts: 114 |
| Location: Bee Hive |
4261.30 Points
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DrugPhreak
Working Bee
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| Joined: 07 Mar 2005 |
| Posts: 114 |
| Location: Bee Hive |
4261.30 Points
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re: Extracting 8% Ephedra
Tue Sep 13, 2005 6:08 am |
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| OK. SWIDP has another pound of 8% Ephedra and this time they are going to steam distill... fuck doing any type of A/B on this shit. This will be done using Biotechdude's version of the Dwarjet, but would an electric coil plate be ok or is using a gas burner mandatory? This will be done with 100gm first just to see how things go. |
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loki
guinea pig
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| Joined: 09 Mar 2005 |
| Posts: 391 |
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14167.88 Points
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re: Extracting 8% Ephedra
Tue Sep 13, 2005 6:22 am |
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| afaik, it just gotta be forced steam distillatio, meaning that you are boiling it while you pass steam through. flames are just very hot and get things up to temperature fast. |
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DrugPhreak
Working Bee
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| Joined: 07 Mar 2005 |
| Posts: 114 |
| Location: Bee Hive |
4261.30 Points
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re: Extracting 8% Ephedra
Tue Sep 13, 2005 7:14 am |
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| On second thought I think SWIDP will just steam distill through their standard 24/40 rig using a short path Liebig with a 3-neck and run a line from the pressure cooker to one of the necks through a stopper with glass tubing. Base 100g of this 8% powder with 700ml 20% NaOH... heat to 95C as the steam is coming in from the pressure cooker... collect 2l... pH to 6 and evaporate the water. They are hoping to get at least 5gm from this small run for a quick nano. This powder looks like cappuccino powder an smells like crap... it's also somewhat salty, but the bitterness can definitely be tasted. Does that sound right to other Bees? |
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loki
guinea pig
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| Joined: 09 Mar 2005 |
| Posts: 391 |
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14167.88 Points
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re: Extracting 8% Ephedra
Tue Sep 13, 2005 7:45 am |
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| the main thing is you MUST have heat under it. ---- can be steam distilled without forcing (heating the flask being steamed) but ephedrine and pseudoephedrine both need forcing to come across and i think ephedrine is extracted this way better than pseudoephedrine. |
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DrugPhreak
Working Bee
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| Joined: 07 Mar 2005 |
| Posts: 114 |
| Location: Bee Hive |
4261.30 Points
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re: Extracting 8% Ephedra
Thu Sep 15, 2005 12:08 am |
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| Actually, ephedrine doesn't steam distill well. Correct? The amount of ephedrine compared to pseudoephedrine in this powder is miniscule though. SWIDP hopes using a 1000ml 3-neck won't fuck things up, but it should bee ~3/4 full a little while after the distillation starts. Of course a 2000ml would bee ideal, but SWIDP can't find a good deal on one right now. Last time they ordered this 8% from another supplier and it was lighter and there was no saltiness... maybe that powder was better. That will bee determined soon. |
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loki
guinea pig
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| Joined: 09 Mar 2005 |
| Posts: 391 |
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14167.88 Points
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re: Extracting 8% Ephedra
Thu Sep 15, 2005 4:14 am |
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it steam distills ok but you GOTTA do it with heat underneath as well as external steam source (forced steam distillation). is the material you refer to have more pseudo than ephedrine? i am pretty sure that ephedrine steam distills better than pseudo due to its greater affinity for water.
i just wish i could get a straight answer about pseudo-only plant sources because precipitating freebase crystals out of cooling naptha is extremely easy to do. i would think just follow a method like the dmt tek's, or better still, something like STBIII... but if its ephedrine, the chemistry of it is different, it is more water soluble as freebase than pseudo. |
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