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Posts 1 - 10 of 10
 
   
    ChimChim9
(Hive Bee)
07-15-01 22:45
No 190789
       Ephedra Extraction Blues    
   
SWIM ground 2lb.s of dried ephedra sinica down to powder.  The powder was then moistened enough to give a paste like consistency.  The mush was then placed in a 5lt short neck Rbf next a heaping helping of sodium carbonate solution 50% was added to basify.  Then the steam distillation rig was set up the flask heated to just under 100 c and the external steam source began pumping in the steam.  The distillate was collected in a quart mason jars.  Well after the first one filled SWIM could see a thin oil layer on top so he addded a little NaOH and the oil layer became much thicker.  SWIM also noticed some cloudy stuff and decided to add some toul seperate and gass.  WTF SWIM's gas was good and dry so was the toul but where in the ? did his freaking crystals go?  Whats more SWIM dropped in HCL with a tad of H2O seperated and evaped.  Damn the shit looked like it was there just like the near finished end product does when evaping, but SWIM will be damned if the whole shebang didn't evap down to zilch!  WTF?  Any suggestions?  I'll be back in a few Gotta drive SWIM over to the Health Food Emporium, again Dohhh!
Was that periodic guide or table? 		 
   
 
   
    terbium
(Hive Addict)
07-15-01 23:58
No 190798
       Re: Ephedra Extraction Blues    
   
Can you expect to steam distill ephedrine? The freebase is soluble in water (1 part in 20). 		 
   
 
   
    Jacked
(Ancient Alchemist Delux)
07-16-01 00:52
No 190808
       Re: Ephedra Extraction Blues    
   
Sodium carbonate will not rase the pH high enough by it self to liberate the FB.
Paid in Full 		 
   
 
   
    Jacked
(Ancient Alchemist Delux)
07-16-01 01:32
No 190814
       Re: Ephedra Extraction Blues    
   
Well I found this in the dispensatory of the US 25th edition.
Isolation of ephedrine from the plant is effected by alkalinization with sodium carbonate or calcium hydroxide and subsequent extraction with alcohol or benzene. The solvent is distilled off, the residue of impure alkaloid is dissolved in dilute acid and, after treatment of the solution wiht decolorizing carbon it is filtered, then alkalinized, and the alkaloid reextracted with ether or a similar solvent. The alkaloid recovered from the ether extraction is purified by crystallization from hot water.

I was wrong about that one
Paid in Full 		 
   
 
   
    Labkey
(Hive Bee)
07-16-01 01:55
No 190819
       Re: Ephedra Extraction Blues    
   
This from my bad memory of the literature: in the 1930's similar processes (A/B) required from 4 to 12 re-extractions to obtain all of the alkaloids (a mixture of mostly ephedrine and pseudoephedrine) requiring further chemical treatment to isolate the two. Low pH has been a problem in the past for ephedra extractions.
How long you been up? Check the calendarlaugh 		 
   
 
   
    ChimChim9
(Hive Bee)
07-16-01 02:30
No 190823
       Re: Ephedra Extraction Blues    
   
terbium - I get your point.  However, SWIM decided to try this technique after reading an old post by oilman 101% return from Ma Haung extract.  Now SWIM has either misunderstood that post or just missed something altogether.  Why would the ephedrine alkyloids carry over through steam distillation with extract yet remain relatively unmoved with the raw plant material?  Are the ephedrines not the same or is the extract ephedrine somehow made more apt for distillation by virtue of the extract production process?   

jacked - Thanks for the info.  SWIM mentioned the sodium carbonate useage for basification so as not to overbasify the goodies.  Although, no tangible data has been located by SWIM giving proof to the possible burnt crispies via loads of NaOH he was just being cautious.  Is burning the ephedrine possible by over basifying?  SWIM has fried some pseudo on occasion.  Dohh!  Also, without asking what kind of alcohol would it be safe to assume that one should use the alcohol that most closely resembles benezene as far as properties go? smile
Was that periodic guide or table? 		 
   
 
   
    Jacked
(Ancient Alchemist Delux)
07-16-01 19:59
No 190968
       Re: Ephedra Extraction Blues    
   
We have been playing around with steaming pills, The NaoH was harsh and blamed in the carmalizing in the pill mash.
Sodium carbonate and a touch of NaoH to bring the numbers up.
SWIM remembers the 101 post and has tryed, Even with heavy basafying using NaoH the results were poor. What came over looked good but failed the burn test. It burnt like wood flakes. 
I hope you get better results than SWIM.

Paid in Full 		 
   
 
   
    ChimChim9
(Hive Bee)
07-16-01 22:06
No 190991
       Re: Ephedra Extraction Blues    
   
Was your steam source internal or external?  SWIM has been using a modified wallpaper steamer.  The steamer works great for extraction of the post reaction product.  Prior to the steamer a pressure cooker was used it was very slow and cumbersome and SWIM spent mwch time waiting.  One more advantage to the wallpaper steamer is that it does not require an external heat source, just plug it in and in about 5 min steam like the Delta Queen.wink
Was that periodic guide or table? 		 
   
 
   
    ChimChim9
(Hive Bee)
07-16-01 22:10
No 190992
       Re: Ephedra Extraction Blues    
   
jacked - was wondering should the plant material be basified with a base/h20 solution prior to alcohol extraction or should the alcohol be basified itself? cool
Was that periodic guide or table? 		 
   
 
   
    dwarfer
(Hive Bee)
07-17-01 04:39
No 191072
       Re: Ephedra Extraction Blues    
   
[b]   

A friend of mine tried the same process: a little different set up, and got some good results.

Real easy: particularly compared to some past heroic efforts, which, although they worked, were tons of work by comparison.

conc. sodium and potassium OH was poured on dried powdered herb to cover.

The material and base was in a glass pyrex container which providentially fit inside a pressure cooker.

the BTU's were added, and the condensed distillate was oily feeling, but an oil layer did NOT form..??..??...??

The pH was (if i recall might be off a bit) 11.6.  That number is suspect since my good buddy whats his name was doing other extractive experiments at the time and might have his #s crossed..

Anyway, NP was added, moderately agitated through recycling of the NP continuously through the aqueous layer, separated, gassed, and found to be quite productive.

The aqueous layer was then pH'ed to 14+: and another separation brought over a fine reddish cast along with a bit more alkaloid: it did not filter out on #2 whatman's.
(damn fine, that ??sediment??)

I think I'll recommend maybe going to pH 13 and no higher for second gasp extractions to see if the reddish cast still manifests.

This set-up was a microwaveable pressure cooker (i did not know they existed either)
..

but it oughta work anywho....

=======

The only time I've had trouble with the "over basification" frying the pre-goodies was when dry powdered -OH was added: then water. Don't know why: or if it has just been luck: or maybe the temp gets locally REAl high then:

but conc. -OH aqueous added seems well tolerated.

Sodium bi carb > sodium (uni) carb @ 100 C: +bubbles

======

alcohol has little merit in steam extraction (at least for me) unless you have a device that will assure the pressurized temp is excess of 100 C.

Such a device can be made by drilling and tapping a hole for a needle valve in a PC:

use a steel braid reinforced hose on the output, then.

the original steam pressure guage then will begin to "pass gas" to alert you that it is time to open the needle valve.

If you choose a braided steel lavatory water supply hose for your output line, you will fine the small end will conveniently fit to one of several needle valve set-ups.

The large end will screw to a male barb fitting which can transition to a decent condenser beter than 'droid's.
AND enable quick and facile disconnnects without tools.

Upon completion of your run, then alky can be poured thru your better-than-'droids condenser to assure that any arteriosclerotic plaques of pre goodie have been deposited in your collector.

Actually, Jacked and 'Droid sent me over here to catch you guys up because they were concerned you were falling off the technological wave:__>__>JUST KIDDING>>>>>....... 		 
   

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