casper (Stranger)
05-23-04 09:52
No 509034
      probs with straight to E     

ok this is what swim did, swim took 200 red hots (exp date was 2004) deredded em added 140 mls of iso, 140mls of napthaput 1/3 over pill mass and boiled 2 mins and did the sam with remaining ext. fluid, wim then added 100 mls of xylene and brought to 105c and boiled and was expecting for suzy to crash out, but got nothing, still got my xylene and extraction fluid, wtf this is first time ive ever done this but i was expecting something to happen what went wrong and what can i do?
 
 
 
 
    geezmeister
(Of Counsel)
05-23-04 20:35
No 509157
      two minutes?     

Did the pills even break up?

mostly harmless
 
 
 
 
    12cheman12
(Newbee)
05-24-04 02:06
No 509194
      okai like you said, this is your first time.     

okai like you said, this is your first time. And like most peoples first time theres going to be big mistakes here.
ISO is used to dissolve the pseudo while Naptha and xylene are non polars which you would be using at this stage to clean your pseudo. Just by reading your post i can tell you didnt follow the steps properly. Im thinking you added the ISO and Naptha together and then boiled, if you did this its wrong. Post in more details of what you did and im sure someone can help you out. But at this stage read the extraction procedure over and over again until you fully understand it and make sure you follow it EXCATLY.
 
 
 
 
    Synthesthesia
(Stranger)
05-24-04 23:00
No 509452
      Something very similiar happened to..     

I just got off the phone with some guy who had read some email from some other guy who said he dreamed about
quote
 someone else taking 3 boxes of 30x96 red balls of shit and boiling them with dried VM&P Naptha and ACS grade ISO. Pills take something like 8 hours to break up. Solution was then vacuum filtered. 150mls of xylene added to solution and temperature brought up to 105C. Solution again vacuum filtered (clean filter), and then washed with 'generous' amounts of MEK. No elfspice in filter paper, but somebody dusted the paper with red shit.

All this on the heels of two failed a/b extractions, but hell that might (must) have been due to wet solvents.

end quote

now my friend is getting emails from the other guy asking what he should do or if he is just a 'big pussy' and that maybe he needs to 'sharpen his game' a little bit.

And if the masses have agreed to split the sea then let it bleed.
 
 
 
 
    casper
(Stranger)
05-25-04 16:06
No 509586
      ok the pills broke up fine, im thinking swims...     

ok the pills broke up fine, im thinking swims prbs is that he did'nt let the naptha iso solution boil long enoung to boil off the iso, after swim let it set for 24 hrs the suzy came crashing out, probably due to evaporation of iso, but! swim wasnt able to filter it hot so some of the gaks probably reatached themselves, what swim is left with is 4.5 grams out of possible 6 of some oily feeling psuedo probably a couple of recrystalizations is in order to clean this?
 
 
 
 
    gluecifer69
(Hive Bee)
05-25-04 18:08
No 509618
      precipitation followed by rextal     


4.5 grams out of possible 6 of some oily feeling psuedo




Follow up with Post 432344 (geezmeister: "pseudo precipitation technique", Stimulants) and then recrystallize for final diamonds.  This should give you quality pfed if it is there and or not got the new methacrylates gakk.

EDIT:Just read your first and according to the exp. date on your red hots, you should be good to go and not have any of the newer gakks.


Scaring the ghosts away
Wake Me when I'm Sane
 
 
 
 
    geezmeister
(Of Counsel)
05-25-04 20:12
No 509650
      sorry casper.     

Sorry Casper. You didn't get the naptha/xylene mix to 105C without boiling the alcohol off. Didn't happen. You didn't extract the pseudo, or enough of it, to start with.

What are you using for a thermometer?

What is in the xylene/naptha mix is not pseudo, its gakk.
It may be a little pseudo and a lot of hypromellose. If it melts into the filter, that's your mixture. Let it melt in the filter. Scrape off only what doesn't melt into the filter and do a pseudo preciptitation in xylene or a 50-50 mix of xylene and naptha.

My guess is still that the pseudo is in the pill mass. Taste it. If its bitter, there's your pseudo. Boil them for a while in a dry alky/naptha mix to extract them, or just extract them with alcohol and pour that in a 50-50 mix of xylene and naptha and heat it up. The pseudo will precipitate out before you ever get to 100C, let alone 105. Filter hot and rinse immediately with MEK.

Be advised that this isn't enough if the pills are loaded with Eudragit.

mostly harmless
 
 
 
 
    casper
(Stranger)
05-27-04 06:58
No 509921
      i am using a candy thermomenter, i dont ...     

i am using a candy thermomenter, i dont understand what you mean when you say melt into the filter?
 
 
 
 
    geezmeister
(Of Counsel)
05-27-04 13:53
No 509964
      what "melts" into the filter...     

Pseudo gakked with hypromellose will form in cooling solvent from the STE, and when filtered out looks clean and white. It will not dry readily, seems to have an affinity for acetone, and as it dries, seems to turn into nothing but an oily spot on the filter. The white powder just seems to "melt" into the filter as it dries.

If your pseudo does this, dissolve it in alcohol and precipitate it in fresh xylene and naptha.  Using the same solvents used to do the Straight to E to do essentially the same precipitation will yield much cleaner pseudo.  As the solvent cools, gakk will precipitate in amounts that might surprise you. You will find the pseudo after this second preciptiation dries faster, reacts better, and doesn't melt into the filters. 

You can see the same melting-into-the-filter phenomenon if  you filter the white powder out of acetone used to rinse pseudo. If what you think is pseudo melts into a filter as it dries, you don't want to put it in the flask. It isn't pseudo, or it isn't clean enough pseudo.

That is what I referenced when I mentioned pseudo "melting" into the filter.

mostly harmless