Author Topic: beautiful  (Read 27660 times)

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spectralshift

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SWIP should have been more precise in his...
« Reply #100 on: December 21, 2003, 10:41:00 AM »
SWIP should have been more precise in his earlier rant. When he went through the trap procedure, he was  v e r y  conservative with the H2O. He did several extractions, and never added more than about a tablespoonfull at a time.

Prepuce no worries, it had little to do with that.
thats a bit troubling.
okay it was clearly a mistake to use NaOH, haha whoa imagine how concentrated it was, I'd bee surprised if much at all survived that.

I have one piece of info which could be relevant to this.
This orange is thought to be a type of PEG right?

A test I did quite a long time ago now with DOt3, a brake fluid, that contains ethylene glycols went like this:

This dot3 fluid normally sits underneath a water layer, just like tetra, dcm, tri or any chlorinated solvent.

So I had Dot3 on the bottom, h2o above, and a NP on top.

Upon basification, most of the ethylene glycols move up to the top NP layer...some different molecular weight glycols remain at the bottom, for possibly 48hrs.

How does this help you? dunno!  ;D  ;D
But what im saying is PEGS don't hang around in basic solutions.
Its possibly not that they change polarity, but rather dont like basic solutions...this is why it can bee washed away with fresh water often/. (ware does this sound right or is it made up bullshit?  ;D )


>>Other than teasing spectral about his choice of usernames

thats okay ware! I don't really like it much anyway, I'm sure that spectralmagic bee isn't too thrilled either.

wareami

  • Guest
Never Fear...
« Reply #101 on: December 21, 2003, 01:40:00 PM »
I wouldn't tease anybee if I didn't have the attention span of a hyperactive rock in a riverbed of polished gems. :P
Oh yeah....and if I didn't like ya!
The troubling gaak is probably a hybrid mixture of povidone, PEG, and polysorbate if Ibee were to make an uneducated guess based on it's behavior and the effects it has on final work-up.

Ibee kicked around the DOT3 in the past and gave UP after not being able to effectively remove the oilyness it imparted to the pinwheels.
It did appear to remove PEG however.
Dwarfer and Ibee discussed this since and the ensueing dialog hinted at giving the DOT3 extraction attempt another crack at a full out Ibee Assault with the addition of an oil remover! You got it! I can hear it now..."Just what we need...more exotic chemicals to play with!"


Its possibly not that they change polarity, but rather dont like basic solutions...this is why it can bee washed away with fresh water often/. (ware does this sound right or is it made up bullshit?)



Geez would be more of an authority than Ibee on PEG and the influence basic environments have on it since his schools of thought surround A/B extraction and Ibee's surround solvent extraction.
Algreich or VE may also chime in on that note based on their expertise with a/b`ing pills.
But Ibee's thoughts would be that if PEG didn't like basic solutions, that would explain why it moves UP with the Pfed into NP, and what you are saying is a water wash of the NP before extracting the pfed from NP would rid it of PEG....Correct?
Now either Geez's trouble with PEG were as a result of staying freebase...instead of going to salt, or this waterwash wasn't employed on NP...
If so...it would make sense!
But...Ibee knows that Geez employs this wash post-rxn based on write-ups and the proposal you suggest would have spared Geez the PEG nightmares of yesteryore that plaugued SWIG's circle post-rxn, ;)  Wouldn't ya think?
Let's see what Geez and the others say before the hyperactive rocks call Ya a bullshitter :-[  ;D  ;) .




spectralshift

  • Guest
:-D ware your hilarious.
« Reply #102 on: December 22, 2003, 01:26:00 AM »
;D  ware your hilarious. Well I'm privilaged then.

Wouldn't ya think?
Possibly..probably. But it's amazing what can be overlooked in the rush.

I should have done better tests, I didn't do water washes of the NP. I do have some more so I might give it a go later...it's probably not very interesting to us anymore, better ways, but it might bee a good wash to follow in ahgreich's trap to remove PEG carrying through to NP.
Depends on results though, get back to ya you PEt!  ;D  ;)

geezmeister

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No NaOH
« Reply #103 on: December 23, 2003, 03:05:00 PM »
Prepuce: Use sodium carbonate to base the pseudo, rather than NaOH. We noticed early on with Orange I and again with orange II that both seemed ambi-polar, but both seemed to become nonpolar soluble at pH levels above 12 to 12.5. Sodium carbonate and trisodium phosphate freebase the pseudo without apparently making the orange gakks nonpolar soluble. NaOH will base too far and the orange gakks will appear in the non-polar. Or so it seems to the cooks who toss more base in for that last pull and get a load of orange death.

The recommendation of sodium carbonate for the base in this application has avoidance of orange gakks in mind. There are other reasons, like ready availability and low cost, but you can't over base the pseudo with it and it isn't going to burn the pseudo if it bases too fast.

I did some work with some 120's and have high praise for Scottydog's comments on ridding the PEG post extraction. The water baths in a small volume of hot dH2O really were amazing. I have a beaker of nasty PEG from the extracted crystals and think the post extraction cleaning is a necessity on the 120's.


elfspice

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vm&p naptha sub in oz
« Reply #104 on: December 23, 2003, 05:33:00 PM »
well, coleman fluid, zippo, etc, i find the brand name ones are more likely to have heavy crud in them but for precipitation crystalisation that's not really a problem. the cheapest source is a solvent called 'shellite' which contains apparently mostly pentane and heptane, and the way it forms microbubbles well before it starts to really boil tells me that's about right. It seems to have similar qualities to vm&p naptha from the descriptions i have read, a solvent you don't get much out of unless it's hot. That can be advantageous if the desired freebase is the most soluble in the material of all the stuff in the mix. (this is certainly the case for dmt)

gas with toluene or xylene, it doesn't matter, so long as they're both dry. xylene can't hold as much water than toluene, which makes it a good choice. Also, xylene is often a fair amount of the content of mineral turpentine, and in my experience organic gak does indeed seem to travel with the residue from the turp, so it's usually worth doing a couple of rinses with some petroleum spirits (whatever form is handy to one)

edit: if you really can't find sodium carbonate, sodium hydroxide+sodium bicarbonate with the right ratio of weight (utfse and get their respective molar weights to determine the ratio) much faster than baking sodium bicarbonate.

Prepuce

  • Guest
Thanks, Geez, Ware
« Reply #105 on: December 26, 2003, 10:00:00 PM »
Thanks for some good tips, Geez. SWIP tried H2O on his FB crystals, but didn't know at the time how soluble they might be and didn't risk boiling it. Obviously he will do so next time!

Getting to be something of a challenging hobby, eh?

Ware: SWIP looked back at your earlier post and his reply, and all he could do was scratch his head. How he understood what he replied to is beyond him at the moment. Must have been the tetra fumes!

PP

geezmeister

  • Guest
Recent water washes
« Reply #106 on: December 29, 2003, 10:00:00 AM »
It is rather hard to take those nice shiny white crystals that are so obviously "only" fb pseudo and boil them in a few cm of distilled water. As the water boils, the pseudo crystals reform and float again at the top of the water, where they may be filtered out. The yellow, oily, turbid water immediately proves that the crystals were not as "pure" as you may have thought. 

At least as to generic 120's, I suggest doing a couple of naptha boils before the tetra trap, or bringing the extracted fb pseudo crystals to a boil in a few cm of distilled water after after extracting them, and repeating such washes until clean.

I wanted to try out Scottydog's evaporation-to-near-saturation-and-decant method of PEG removal, but the number of strangers in the neighborhood walking around in the still night air dissuaded me from doing it this time. out,
The tetra trap can be used to extract fb pseudo from generic time release 120's if one first does a series of naptha boils to remove PEG from the pill mass, or alternatively washes the fb crystals in boiing hot water a time or two.

The final product is like-you-like-it.


spectralshift

  • Guest
So is that little crit ahgreich coming back?
« Reply #107 on: December 29, 2003, 05:44:00 PM »
So is that little crit ahgreich coming back?

>>bringing the extracted fb pseudo crystals to a boil in a few cm of distilled water after after extracting them.

I remember that idea--oh yeah it was my own!  ;D  :P

geez SWIM had the same problem as you actually doing it, luckily Scotty is more care-free.
I still don't know about it on paper, are you sure none of the fb gets steamed off?

maybe inside a weighted tea-bag would bee safer, as it's being brought up to the boil?

Also depending on what the end concensus is about ethyl acetates safety, being used in a similar way..maybe it would bee an even cooler solvent to use in the same way. But Os and Kinetic have to talk more first.  :)

wareami

  • Guest
For what it's worth...
« Reply #108 on: December 29, 2003, 06:36:00 PM »
Not that methods of boiling aren't useful and effective for removing gaak and unwanted intermediates, but care really should be taken whenever pfed or meth are brought to boiling points in any solvent without the use of a device to capture the goodz.
It's always been easy for Ibee to associate yield loss with boiling and that atmospheric pfed/meth addict in the attic!


geezmeister

  • Guest
some loss
« Reply #109 on: December 30, 2003, 12:46:00 PM »

I still don't know about it on paper, are you sure none of the fb gets steamed off? maybe inside a weighted tea-bag would bee safer, as it's being brought up to the boil?




I most likely lost part of the pseudo yield to the hot water baths I gave it. There was the smell of pseudo in the room after doing it, and there certainly less of a pile of pseudo after it finally dried than there was before I water-washed it. I reduced the wash water over low heat to precipitate any remaining fb as crystals until no more formed. No additional crystals formed in the cooled solution.

My attempts to steam distill pseudo have met with limited success at best, which suggests to me that losses to boiling should not be that severe. I did have a loss in yield, though. Washing in hot water does clean the fb crystals, however, as demonstrated by the superb quality of the final product. I wonder whether steam distilling the extracted freebase crystals might be in order, rather than steam distilling from the based pill mass.

I think that I need to steam distill my next batch of fb crystals and compare losses to boiling and filtering. Might be a real answer to the yield and purity issue, particularly if it is easier to do than steam distilling from based pseudo tablets.

Have you noted a difference in yield when boiling in a tea bag?

The cleanliness of the washed pseudo is is worth some loss in yield, in my opinion.  The quality of the final product damn sure bears that judgment out. I think it may be a matter of limiting the losses in yield, rather than wholly avoiding them.




spectralshift

  • Guest
Re: I most likely lost part of the pseudo...
« Reply #110 on: December 30, 2003, 02:14:00 PM »

I most likely lost part of the pseudo yield to the hot water baths I gave it. There was the smell of pseudo in the room after doing it, and there certainly less of a pile of pseudo after it finally dried than there was before I water-washed it.




Dsmn. that sounds pretty conclusive.


Have you noted a difference in yield when boiling in a tea bag?

No no I'm just thinking through ways to avoid the yield loss.
I don't think it would change much, though it might.
because when you boil the crystals at the beginning from on top of the water, steaming is arising from beneath them before they are dissolved.

In a tea bag it might help matters. But you wouldn't know when they had dissolved.

Ware your probably right in your observations.  ;)


weaz1dls

  • Guest
Place a funnel
« Reply #111 on: December 30, 2003, 02:41:00 PM »
Place a funnel on the top of the beaker/carafe and with gloved hand move beaker in circular motion to swirl contents for stiring.  Funnel acts as a makeshift finger condenser. SWIW uses one in the micro, acts as a splashgaurd for bumping. ;D

geezmeister

  • Guest
two clean 120's extractions
« Reply #112 on: January 05, 2004, 08:03:00 AM »
SWIG grabbed more 120's to test a couple  of ideas that might make the tetra trap yield PEGless pseudo. the 120's SWIG gets are loaded with PEG and Orange, so badly that he at one point quit buying them entirely.

One batch he soaked overnight in xylene, then brought that up to almost boiling, let settle and decanted the xylene, then added naptha. The naptha was heated with stirring until it first began to bubble, then removed from heat and the pill mass allowed to settle, and the naptha decanted. This step was repeated. The pill mass was then rinsed with acetone to help remove the remaining naptha, and the pill mass spread out and allowed to dry. After it was dry, it was mixed with Na2CO3 and ground in a coffee grinder and the pseudo extracted by the tetra trap method into three volumes of naptha. This naptha was allowed to cool to yield freebase crystals which were remarkably long and slender, burned with no trace on aluminum foil, and produced methamphetamine witn no trace of PEG, Orange I, or ORange II.

A second batch was processed without the naptha boils, but pseudo HCl was obtained by gassing the naptha used to extract. SWIG used 91% ISO to mobilize the NA2CO3 in the tetra trap method. He did this twice, then gassed, obtaining pitiful yields of pseudo that vaporized fairly cleanly on foil. A third pull was done of the pill mass, this time using water to mobilize the base. This pull yielded very well, making up for the low yields from the earlier pulls. Vaporizing this pseudo on foil left almost no trace unless the pseudo was overheated and burned. All pseudo HCl obtained by gassing will be recrystallized before being reacted, and SWIG will report whether he discovers any nasty surprises with this pseudo.


spectralshift

  • Guest
ahem..
« Reply #113 on: January 05, 2004, 10:41:00 AM »
It's not really the quality of the pfed that makes it through to the non-polar that's in question. It's the lost yield in the event of orange being activated.

Orange gak won't follow through because it is barely if at all soluble in NP's.

 

Alright so alcohol is a no GO(!)er  :( , I guess it does make sense when you factor in that the NA2CO3 is hygroscopic, so even if it is saturated by gak for the process, then it will still leech it's water.

It's a pity though...nice experimenting geez!

SHORTY

  • Guest
Methanolic 'Tetra Trap' worked for me
« Reply #114 on: January 05, 2004, 01:02:00 PM »
I decided to give methanol a try and was surprised at the results.  I started with 199 white 60's w/trip.  All pills were placed in a blender along with an equal amount of sodium carbonate and a teaspoon of tri-sodium phosphate.  The tetra trap was followed using methanol instead of water.  Xylene was the np of which three pulls were done each of which were gassed seperately.

The three were then combined and more methanol was added to dissolve the pseudo and then placed on hotplate.  The xylene was then heated to 105C with occasional assistance of a blow dryer to speed up the precipitation of the pseudo.

When the temp reached 105C the beaker was taken of hotplate and the needles allowed to settle and then the xylene was carefully decanted and acetone was added, stirred and decanted 3 times then left to dry.

Final yeild of pseudo hcl was 9.95g (83.3% yeild) of pseudo which left no residue when heated gently on glass.

The whole process took less than 2 hours.


spectralshift

  • Guest
Fancy that
« Reply #115 on: January 05, 2004, 04:34:00 PM »
ShORTY that's brilliance! WELL DOne man!
nfi how it worked though because now looking at the merck entry for carbonate, it's 'insoluble' in alcohol, what do you reckon happened?

Awesome, awesome yield shorty, very respectable.

There's 17.7% you were robbed of Shorta, are you going to add another trick for the next experiment or leave it as it is?
8)  8)  GO SHOrTy!  ;D  :)  :)

gluecifer69

  • Guest
Great Work Shorty
« Reply #116 on: January 05, 2004, 04:43:00 PM »
Shorty, Geez, and Spectral all contributed to my first post and Gluecifer69 learned more from that than he had in two years of following lokal "cook".

Sorry for the ass kissing, but this is a great break through in Gluey's opinion as Gluey is a fan of the tetrasnare.


SHORTY

  • Guest
Im gonna give acetone a try
« Reply #117 on: January 05, 2004, 08:49:00 PM »
I think i will try acetone next time.  I think the other 17% was still in the pill mass and i might have been able to get more of it with one more pull.  However, i didn't want to risk pulling alot of shit with it and was out of xylene anyway.  Even if i can't get more than 83% it still beats previous attempts on these pills by at least 23%.  So i am content with the results for now.

I also just noticed that the decanted xylene is full of snotty looking gaak. Alot of it too!  Don't know what it is but there is alot of it.  Must have precipitated after it cooled.  I have found that if the xylene is filtered rather than decanted, this shit will get stuck in the filter and is a bitch to remove from the pseudo.  I lost a few needles in the decanting stage but hardly enough to be concerned with.


gluecifer69

  • Guest
Evaping too quick?
« Reply #118 on: January 06, 2004, 07:41:00 AM »
Gluecifer has been struggling since the beginning to make 50% returns on the tetratrap.  He usually gets between 35% and 40% on average.
    Could he be evapping too hot and quick, thus losing some pfed?  Gluey followed Ahgreich and ScottyDawg's write ups verbatim.


geezmeister

  • Guest
basing using acetone or alcohol
« Reply #119 on: January 06, 2004, 07:41:00 AM »
When I was trying to figure a way around PEG in the straight to bee extraction method, I found that mobilizing the base with anhydrous acetone, or a mix of anhydrous actone and methanol helped reduce the PEG in the pseudo extracted. Acetone and alcohol both work well with NaOH, despite protestations that water is necessary with NaOH. The same was said to be true of sodium carbonate, but in actual trials I found that alcohol, acetone, and combinations of both worked to mobilize the sodium carbonate. In the straight to bee, the pill mass was dried after basing to evaporate off these solvents after the base was mobilized.

ISO can be used, but is not as effective as methanol or acetone. I thought that the small water content of 91% ISO might make using it advantageous in the tetra trap; it would avoid using very much water in the extraction--I had hoped it would be enough to aid the basing process without being so much as to become a problem. It did not appear to work very well. Shorty's post makes me wonder if a little water and methanol might not be a better combination for this purpose than the 91% ISO. It may be that using a very moderate amount of water is helpful, and may increase yields over waterless methods, if the amount of water is limited enough to avoid problems with the pill mass. Acetone that has not been dried might serve the same purpose.

Shorty-- that is as high a yield as I can recall having or reading about for an a/b extraction! You might try doing this with methanol and a little water-- similar to what I tried with 91% ISO. If you do it with acetone, you might also do it with acetone that has not been dried to see if the yield may be a little better. I have the sense that adding a little water during the basing process will improve yields. Tetra's presence in the GUPs initially prevents the water from activating the gels and other water-activated gakks that would otherwise be yield killers. The water is advantageous to a point, but once past that point it limits yields. Perhaps methanol with a little water, or acetone and a little water, or an acetone/methanol
mixture with a little water would improve yields. Perhaps using acetone straight from the can, without drying it, might be better than dried acetone. The same might be true of the alcohol used.

I like the way you avoid filtering by decanting the nonpolar and rinsing the pseudo with acetone multiple times. You commented: "The decanted xylene is full of snotty looking gaak...  Must have precipitated after it cooled.  I have found that if the xylene is filtered rather than decanted, this shit will get stuck in the filter and is a bitch to remove from the pseudo."  My question is whether you would have this in the filter if you filtered the xylene hot, at 105C, before it cooled enough to precipitate the snotty gakk?

Spectralshift: your comment that "It's not really the quality of the pfed that makes it through to the non-polar that's in question. It's the lost yield in the event of orange being activated. Orange gak won't follow through because it is barely if at all soluble in NP's."

I disagree. Getting the pseudo without getting anything else is the whole point, and orange isn't the only enemy.