New Straight to E -- a novel extraction tech.

[MnkyBoy78]

SWIM doesn't filter the Naptha/ISO...Just lets it settle for ~20 min.  The Charmin Plug used for filtering the Naptha/ISO/E solution is tightly packed, hence the use of the vacume pump.

[ChemNewbie]

That's the clean Pfed my man. Don't throw that shit away, or you've wasted your time. When clean pfed is crashed out of a NP solvent by gassing, cooling, or any other method, it will usually have an "applesaucy" appearance while still in suspension in the NP. Once the pfed is filtered and dried, if it is clean, it will often have a cotton-like appearance. The cottony look simply means that the crystals were crashed out of the NP in a rapid fashion, and are very small with little air pockets between them, making them look fluffy. If you want big crunchy crystals, try dissolving the cottony ones in boiling ISO, add a little acetone to the alky, and allow the solution to cool very slowly, over the course of several hours. This re-xtalizing procedure will remove even more impurities, and will often leave the perpetrator with thick nail-like crystals which will readily reduce to our favorite amine in a HI rxn.

CN

[joe420]

I thought maybe it was cause it was sol in h2o but not in naphta but tried to recrystal and got nothing .... and there was way too much of it ! weight and was 12gram when should have been at best 6.5-7gram ! have not tried jap dry and i can't locate it

[beez_neez]

Hello childeren,
                  If you are an oz bee, and are having difficulty locating japan drier, it is probably because it dosen't exist here in our neck of the woods. Well actually it does, it's just called something different!
We here, down under, like to call it 'terebine'. Available from all leading paint stores as a drying accelerant for oil based paints.
A little research has turned up the following:
Terebine:
72% liquid hydrocarbons(mineral tupentine)
14% cobalt octoate
14% manganese octoate
From what Swibn can gather, this has very similar properties to the jap stuff.
Swibn is about to run out and grab some as well as some MEK and give it a go on some der...der....you know what-azin.
Shall post results soon.

[Osmium]

> 14% cobalt octoate
> 14% manganese octoate

You people use that crap to extract pills???
One question: WHY???

[beez_neez]

Os, but to remove the orange nasty before utilising your favourite extraction method.

[beez_neez]

JAPAN DRIER (lead free)

 Used by the Professional Painter,  Japan Drier is a special blend of petroleum hydrocarbons and a combination of high quality drying agents.  This blend of agents accelerates the drying process of oil based paints and coatings.
When faced with damp or cool climate this product is very effective when mixed with paint to speed up the drying time between applications or touch.   The lead free driers are the same basic driers used to produce paints, including Cobalt and Manganese.  Use 2 to 4 ounces per gallon of oil-based paint or varnish and mix thoroughly.  Always check and follow paint manufacturers recommendation for thinning. 
READ MATERIAL SAFETY DATA SHEET BEFORE USE

[geezmeister]

Why JD?

I have used it diluted in naptha, boiled the GUPs in it, then boiled with naptha again and then twice with MEK. The pseudo so obtained had none of the persistent orange gakk that has plagued me this year.

I then diluted it 1:10 (I believe it can be diluted much further) in MEK  and did a microwave solvent boil of the gups in that solution, and had the same results.

It seems to break the newer gaks into components that can be removed with standard solvent boils or microwave boils prior to extraction of the pseudo. Haven't found anything else that works as it does.

[halfkast]

I'm having a feeling that n,n,n-trimethylbenzene could bee doing some or all of the cleaning work.
It's included in lots of Japan Driers but not terebine...

Though if this is the case I'm sure the task of finding something is even more simple.

[barkingburro]

been a long time in hiding but swibb inadvertantly seemed to bypass the orange II (poly-pyropovirolidone?). unless he's just balls to the wall lucky and/or crazy an 100% ipa extract just after solvent boils and subsequent re-xtal rather than evaporation seems to shed the sticky shit. granted swibb's %'s have been affected as the crap gets more and more concentrated towards the final pulls from the ipa. maybe swibb has just gotten good pills. but we are talking about the green 24/60's one might target in a redish super store?

[geezmeister]

No, you are wise and fortunate in your pill selection, barkingburro. Stray from those to the more heavily gakked versions remaining on the store shelves in my territory and the orange will bite with even sharper teeth. Those pills don't even make it to the shelves where I live. They disappear out the back doors of every retailer for twice the shelf price, paid in cash, with promises of more the next time.

[Osmium]

I'm just wondering why anyone would intentionally contaminate their precursors with toxic, hard to remove heavy metals and complicate the whole deal by adding yet another component to the max and another variable to the equation.

[SHORTY]

Are you keeping the secret to the removal of the orange gaak to yourself??? 

Obviously, there should be better, less toxic methods to remove it. Unfortunately, we have not found such a method so therefore we use what we can obtain in order to get clean psuedo.  What pills do you use?  Have you had to deal with the orange gaak I or II and if so then how did you do it?

[aussie2]

http://www.tricoat.com/pdf/d404.pdf

[barkingburro]

ok, swibb took the plunge and deviated to time release 120's just to try this method. impressive. was slightly concerned at first cause swibb didn't follow directions as he should have and didn't hit 105. swibb also had concerns about the psue as it looked different upon filtration than his evap/crashed psue norm. upon rextal in ipa 100% all looked well. something to note however, maybe it's just swibb's manhandling of his dope, but the yield rate seemed to be lower the smaller the number of boxes porocessed. as a test swibb tried 1 box and had a 40% return, tried 3 and got 70... maybe swibb just gets lazy with small amounts of dope, or maybe a minimum amount of psue will always be lost due to things like adherence to the beakers, etc.

has any-one answered the dry matrix formula question yet? i couldn't find an answer.

wow, it's really cool not haveing to resort to long evaps to preserve yield. speed chemists being patient... ha there's a dichotomy for ya. thanks again swive. hope you don't live near swibb and i feel for any competitors that do. not that any-one ever does this sort of thing for money or anything... ya, ok... bok bok

[halfkast]

>>maybe swibb just gets lazy with small amounts of dope, or maybe a minimum amount of psue will always be lost due to things like adherence to the beakers

That is loss that should never happen, as it's the loss that is easily avoidable.

Yes you are quite lazy.  

has any-one answered the dry matrix formula question yet? i couldn't find an answer.

So where did your 120s come from, Transylvania?

How do long evaps "preserve yield" ?
Invariably clumsy are we?  

[barkingburro]

now i take offence to that one . lazy, yes at times, but clumsy, no. by long evap i mean as compared to an evap with heat. ergo, a long evap with no heat will yield more than a short evap WITH heat.

ok, so the transylvania comment meant what? are 'extended release' by nature all dry matrix? if so that's a new one to me...

ok and onto some other observations with straight to e...

it would behoove any bee to test one pill or one box of pills before going without a grinding of the pills. swibb encountered a batch of 60's sold in 48 packs and with tripdoline that did NOT dissolve/disentigrate during the boil. yield ended up at about 50% after reprocessing, and there seems to be more lurking but the whole thinik looked like a helluva mess from where i was sitting.

[awayman]

Could you please help with swims yield problem? Swim uses this method and is very happy with the quality product that is achieved. However, his yields seem a little low. 70% is tops on the comeback. He followed the procedure to the letter as he has every time since it was first posted. (Well done by the way)The only thing that swim notices is that some of the pills are not dissolved and still maintain the original round shape (white 60's), could it bee the time he boils the extraction liquid and the pills is to short and he needs to let them boil longer before pouring off and adding more extraction liquid? Swim is leary of scorching them and ruining the whole damn thing. Any help would be appreciated.

[geezmeister]

Awayman: you won't hurt anything by crunching the pills up with a pestle or grinding them in a coffee grinder. If they are not dissolving, you probably are leaving a little pseudo behind.

The yield will be dependent on the inactives present to a degree. The cleaner the pills, the better the yield. I've gotten as high as 98% from generic white 60's with two listed inactives and gotten clean pseudo. There is one generic I have gotten 98% from, and it has six or seven listed inactives. The generic 120's have not yielded cleanly for me by this process, and the yields from them when they are precleaned have been in the typical 60% range.

One other thing to keep in mind is that once that alcohol/naptha solution is boiling, you are rapidly losing the alcohol. Boil too long and you reduce the alcohol you have available to dissolve the pseudo, have mostly naptha and maybe not quite enough alcohol. I did that the second on third time I did this process, went back and boiled the GUPS with more alcohol/naptha solution and picked up the missing pseudo.

VE's point was that you don't HAVE to grind the pills. It was not that you SHOULD NOT grind them.

[barkingburro]

well, swibb will concur with geez on the generic 120's. yield after shedding polysorbate 80 is back down to 40% on them... any ideas on how to shed it b4 the straight to e? if i'm correct then polysorbate 80 is only in the outer jacket of these 120's. any ideas?

the generic 60's... 2 for 2 have needed a grinding prior to processing.