Author Topic: Fucked up ephedra steam extraction  (Read 2478 times)

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place

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Fucked up ephedra steam extraction
« on: March 01, 2004, 12:13:00 AM »
SWIM hate those plantshit  ;)

Friday, SWIM tried to make a steam extraction of ephedra 8%. After trying steam extraction 350g ephedra 8%  he learned that it is important that the flasks are big enough :-(  Max 50-100g ephedra 8% i 300mL water in a 1l. flask.

After the first accident he tried again with only 50g in 300mL water. The system worked fine, but the result was only water, no freebase ephederine. There was one problem. How can SWIM make sure that the water + plant is base? pH 14. He tried to add a solution of 100g NaOH in 500mL water, but he couldn't read the liquid with his pH papers, because the ephedra brown plantshit coloured his papers totally brown, so there was no colour to read after.

Is there anyone who can help?


DrLucifer

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Simple
« Reply #1 on: March 01, 2004, 12:23:00 AM »
All your problems can be solved with practice and a digital pH meter,  :P  $100 will buy you a good meter with a 0-14 range, maybe even a 12 month warranty!
May i suggest that you start small and work your way up, dont want to be wasting any more herb!  ;)


Bandil

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Try filtering through a glass frittet funnel...
« Reply #2 on: March 01, 2004, 02:51:00 AM »
Try filtering through a glass frittet funnel (or a normal funnel w. filter paper) a small sample and read the pH of that...


biotechdude

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Never fear, ya mamma is here
« Reply #3 on: March 01, 2004, 03:11:00 AM »
he learned that it is important that the flasks are big enough

Indeed, you DONT want to overload the flask.  NEVER go beyond half full otherwise foam and bumping will FUCK your distillate.  One drop of crud can kill purity. 

Swix uses these ratio using proper distillation glassware - 100g powdered plant, ~600mLs water, and adds the caustic powder directly (and slowly) with heavy stirring.  This sludge turns out to be about 800mLs in total.  This is added to a 2Ltr rbf.

but he couldn't read the liquid with his pH papers, because the ephedra brown plantshit coloured his papers totally brown, so there was no colour to read after.

EXACTLY, and wally world digi pHers wont cut it either and the crud dirties the membrane and gives unreliable readings.

To rectify - when you have the well mixed plant/plain water slurry...Swix adds raw caustic powder in sprinkles and it starts to get gummy and black and a bit stinky.  You keep adding caustic until the thick solution THINS out again and it is really black and almost makes u puke cos it smells really strong and fishy/basey.

Now, just boiling the flask and generating internal steam CAN work using vacuum and a vigourous controlled boil.  However, the volume will go down, and if using 100g of 8%, the 400mLs or so that u could bring over without running dry, probably wont be enough to carry all the goodies.  Also, as the volume decreases, more microscopic crud will come over.

Conversely, external steam (superheated even better) will carry the freebase better.  Secondly, you can keep collecting distillate (and ALL the goodies) and the flask volume will stay the same (as long as you keep it at ~95c).

Hope that helps...

place

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That was exactly was happened :-S SWIM tried...
« Reply #4 on: March 01, 2004, 05:56:00 AM »
NEVER go beyond half full otherwise foam and bumping will FUCK your distillate.  One drop of crud can kill purity. 

That was exactly was happened  ::)

SWIM tried to filter the liquid with lab filters, but was not possible; the brown shit simply would not go away. Even a small drop and the pH papers were fucked.

Biotechdude: SWIM used to flask, one with steam and one with plant. It was easy enough to get the oliebath in the steam flask to work, but it was pretty hard to keep the plant flask under the 100c. Every time the hot steam was bubbling up, the water and plant started to boil.

What is raw caustic?

Would it be possible to make a dH2O solution with NaOH ph 14 first, and then afterwards put the ephedra powder in? Or will the burn up all the ephedrine?

rgs, place


auntyjack

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i think it was dwarfer who sugested it but...
« Reply #5 on: March 01, 2004, 11:52:00 AM »
i think it was dwarfer who sugested it but sand is an excellent filter for ephedra extracts


biotechdude

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more troubleshooting
« Reply #6 on: March 01, 2004, 01:56:00 PM »
SWIM tried to filter the liquid with lab filters, but was not possible; the brown shit simply would not go away. Even a small drop and the pH papers were fucked.

Well u dont NEED it to go away.  Setup correctly, the brown shit doesn't interfere and the distillate is clear.  However,  sand filters would remove alot of the microscopic plant crud and increase your safety net.

Biotechdude: SWIM used to flask, one with steam and one with plant. It was easy enough to get the oliebath in the steam flask to work, but it was pretty hard to keep the plant flask under the 100c. Every time the hot steam was bubbling up, the water and plant started to boil.

Oilbaths probably aren't the best heat source in this scenario.  That is because (as u mention) the steam entering the system messes with the temps; and oil baths are too slow to counteract.  Swix would recommend a gas stove to heat the flask. 

Also, how did u find the steam flask?  Sometimes they can be hard to either get going or slow down.  For this reason, Swix used one of those little steam cleaner units....They allow control over steam flow and its steam is generated under pressure (meaning its HOT hot hot)... Make the connection from the steamer unit to the flask as short as possible for the same reason.

What is raw caustic?

Caustic - Lye, NaOH powder...the shit u use to make your NaOH solutions. 

Would it be possible to make a dH2O solution with NaOH ph 14 first, and then afterwards put the ephedra powder in? Or will the burn up all the ephedrine?

Yeah it will prob run the risk of frying it. 

Really dude this is quite easy.  Just powder plant, mix with water.  THEN add NaOH (either powder or conc. solution) slowly (so it doesn't fry) until it smells really bad and is a black motor-oil like consistency.  Then put it in an efficient controlable steam distillation setup.  Done.

Newton

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Re: Would it be possible to make a dH2O ...
« Reply #7 on: March 01, 2004, 02:54:00 PM »

SWIM tried to filter the liquid with lab filters, but was not possible; the brown shit simply would not go away. Even a small drop and the pH papers were fucked.




Been there, done that. Once some of the brown gunk has boiled over into the receiving vessel, there is no way to seperate it from the ephedrine/water solution. Only way is to start over and allow for larger safety margins this time.

Edit: Just to clarify- I was talking about stuff  which has accidentially boiled over (Ephedra plant matter/ NaOH solution).
The brownish stuff which comes over even with a correctly done steam distill can be removed with a simple actone wash of the ephedrine salts recovered after acidifying and evapping off the destillate. A dual solvent recrystallisation from water/acetone is even better, it will yield sparkling white crystals.



Would it be possible to make a dH2O solution with NaOH ph 14 first, and then afterwards put the ephedra powder in? Or will the burn up all the ephedrine?

Yeah it will prob run the risk of frying it. 

Really dude this is quite easy.  Just powder plant, mix with water.  THEN add NaOH (either powder or conc. solution) slowly (so it doesn't fry) until it smells really bad and is a black motor-oil like consistency.  Then put it in an efficient controlable steam distillation setup.  Done.




Well, putting the ephedra powder into NaOH solution doesn't hurt it. SWIM does it all the time. On the other hand, he always avoided adding powdered NaOH to the water/Ephedra sludge, felt like _that_ would burn the ephedrine.
But since Biotechdude has tried that, both ways seem to be fine.


place

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Well, SWIM think that his setup is ok.
« Reply #8 on: March 02, 2004, 08:54:00 AM »
Well, SWIM think that his setup is ok. When I took off the hose to check the steam, lots of steam came out and when I put back the hose, the system was closed (no steam out).

SWIM give it another try  :)


Newton

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One more piece of advice...
« Reply #9 on: March 02, 2004, 10:54:00 AM »
Every time the hot steam was bubbling up, the water and plant started to boil.

The water/plant mixture probably didn't 'boil' in a physical sense, that is undergoing a phase change from liquid to gaseous.
The 'boiling' or more like 'agitation' of the mixture was caused by the introduction of a water vapor. More on that later...

SWIM used to flask, one with steam and one with plant. It was easy enough to get the oliebath in the steam flask to work, but it was pretty hard to keep the plant flask under the 100c.

Why would you want to keep the flask with plant/water mixture below 100°C? The solution has to be at its boiling point, otherwise the introduced steam (unless superheated) will condense when introduced to the mixture instead of passing it, and carrying over the ephedrine. That explains why none was found in the reception vessel.

The flask will also lose heat at its surface, causing water to condense, increasing the solution volume. This has to be counteracted by _heating_ the plant/water vessel, in order to keep its liquid volume constant.

To make things worse, the boiling point of a concentrated aqueous solution at atmospheric pressure is _not_ 100°C, but can be significantly higher. For example, the bp of an aqueous 20% (by weight) NaOH solution is 108°. Soluble components introduced with the plant matter would increase the bp even more.

So heating that flask in definitely in order, unless superheated steam is used. For a 1l rb flask SWIN uses a heating mantle set to 100W power with good results.
For your setup, the correct amount of heating can be determined to observing the volume level in the water/plant mixture flask - if it increases, more heating is required, if it decreases lower the heat.

place

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When using E from ephedra 8%, is the portions...
« Reply #10 on: March 04, 2004, 10:29:00 AM »
When using E from ephedra 8%, is the portions so still 1:1:1/3, I:E:rP?


dwarfer

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do this
« Reply #11 on: March 04, 2004, 12:09:00 PM »

Post 488247

(dwarfer: "The DwarJet: a superheated steam extractor", Stimulants)


except have two internal flasks.  one with the ephedra material in strongly basic water, with the "steam in"
glass tube to beneath the water level near the bottom

and the output short tube connected to another identical
flask set up that is empty.  the second flask has it's output directe to the needle valve.

the only use for the second flask is to catch "burps" or foam that might otherwise mess up the works.

Usually, you can forget about it.   Your steam thruput
can be maintained at a fairly lo level without sacrificing steam-extraction efficiency, as compared to other designs
which require balls-to-the walls process speeds since their
mechanisms are radiating heat to the environment at a
prodigious rate. 

Because the entire device is inside the PC, you can go slowly enough to not have foam or splashes cause a problem.

Weight the flasks or elevate them so they won't float...

=============

I gotta take some more pictures.. :(


Offline CooksHelper

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Re: Fucked up ephedra steam extraction
« Reply #12 on: February 28, 2016, 09:07:27 AM »
Would simple methanol extract then using 1/3 sodium carbonate with 2/3 koh using 50grams powdered mu Huang in 400 mills dh20 allowed by use of somewhat dwarjet design just using one of household steamers  instead of pressure cooker (awesome ideas from both dwarfer and biotech mentioning the household steamer for I just so had one so with one failed attempt here comes the glass) this in a 1000 ml 2 ltr rbf run through simple distill for 1.5 hrs first 30 minutes at 95c then over hour allowing  slow  never allowing more than 135c if possible to 150c at a period of 5 if reaches that high of degree then allowing to cool t al clear and save redistilling previous by just read a simple a/b in said case using leftovers and slight amt fresh sodium carbonate mand koh to see if all was extracted ....... Ty guys u are intelligent awesome men

Offline Tsathoggua

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Re: Fucked up ephedra steam extraction
« Reply #13 on: April 09, 2016, 06:33:27 PM »
Simply powdered ma huang? or that dark extract stuff? the latter is a total wanker to deal with.

And as far as PH meters go, a perfectly decent one with a glass electrode can be had at auction online for next to nothing. Tsath's old one came from china. He needs a new one though, after something ate the electrode.

For purified isolates still full of muck, sublimation in vacuo onto a coldfinger,( or kugelrohr distillation, bulb-to bulb short path distillation) of the base, of the contaminated yield of eph/phed/noreph/norpfed after removing the remaining water in a dessicator


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Offline ricky

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Re: Fucked up ephedra steam extraction
« Reply #14 on: April 09, 2016, 11:35:57 PM »
A pH of 14 is insane. Since amine groups are basic, a pH of 12 or so should be sufficient. A pH of 14 would be 100X this. I'm not sure what pH may cause oxidative problems i.e. deamination. For acid when protonating the amine, a neutral pH is enough.

From the OP (I know it is old) it almost seems like it might have worked in the first place. You would probably obtain an aqueous solution; due to the extra OH group and subsequent H-bonding and charge distribution, the freebase might be too soluble in polar solution to crash it out.
« Last Edit: April 09, 2016, 11:39:21 PM by ricky »