Oops grabed the wrong solvent, think again!

[weaz1dls]

Props to Wareami sharring info on Laquer Thinner in a PM.

Just now slowin down after awaking from a twisted dream.
This post shared as a template or spring board for yet more atacks for the gaacks.

Bare bone steps;
     a)grind
     b)Alc pull/filter
     c)reduce vol
     d)precip in LT (Laquer Thinner)
     e)filter/rinse    
 Ok let the scoffing begin! SWIW found swiw's self with no acetone, a small bit of denatured, small bit of xylene, no drying agents (salt, mag-sulf). And way beyond unwilling to venture out for ANYTHING.  Swiw's tweak melon was sure a procedure with what was availible existed and would hear of nothing more. Originally had in mind to xtract np from the LT to use on a A/B with ISO/Denat.  Ya right!  Would aparnetly rather climb a greased pole rather than take a set of steps to get upstairs too!  Remembering Wareami's PM saying to make use of a mistaken purchase of LT rather than acetone and that LT in combo removes oranges and such, will let him share his findings.  Don't want to possibly spoil his next writeup.  The can says contains Acetone, Alc's,Ketones,Esters,Glycols,Pet- Distilates,etc.  Swiw decided to give it a go as a premixed solvent like mixing NP and Alc to precipitate.
   SO;
       a) 8 box generic 120's ground in blender 90sec
       b) aprox 42oz ISO & +/- 2oz Denat added w/stirring
       c) Heated in micro more stiring (no boil)
       d) Suction filter 2 times first 2ply charmin
          plug topped with cotton plug lightly!-packed and
          topped with 2 cotton disk pads. 2nd filtering
          w/4plys plug packed tight cotton pad on top. When
          all alc had been decanted on first filtering,
          the GUPs n all were poured int the fliter and
          and rinsed w/more ISO then left over sucction
          filter.  THen GUPs were put in ziplock just in
          case. (C.Y.A.)
       e) Reduce mix down to aprox 6 fluid oz. Want to
          keep the denaturants free flowin and shift the
          soulubility of psuedo down.  Tone seems to
          act as and open invite for psuedo to disolve with
          orange present unless used in large amounts
          quickly only to reduce loss not stop it.
       f) In a tall caraffe/64oz+ beaker add LT (Laquer
          Thinner) Boil out tone/alkies in micro Swiw
          added about 20 oz to the reduced 6oz mix. Mix
          began turning yellow as volume decreased. Micro
          was intermitent with hand swirling to release
          built up energy, not to fond of bumping! Mix 
          will reach a point where it sounds like
          sizzling  bacon. Remove from micro and swirl.
          POW!, instant oatmeal. It needs to remain just
          soupy enough to flow. Suction filter through
          nonpacked cotton. SWIW poured the filtered fluid
          back through to catch some of the precipitate
          forming inside filt flask.Try not to let the
          pseudo dry out before rinsing with the xylene.
          Then SWIW let sit and packed down filter cake
          while suction dried. filter cakewas incredebly
          clean.
          Rinse w/xylene
          Leave in filter under suction

  Burn tested on glass and even stood up to slight over heating w/out discoloration.  Some black left behind though...In hind sight is was prob more sulfates from galssware than anything. seing the result SWIW got greedy and went for the mix in the rinse slop.  BAD IDEA!!! (Bastard slugyfed)The first filter cake weighed in at 19.36g after drying out in the oven til bone dry. This was thankfully split into two piles as swiw forgot the bastard collection in the filter-funnel. One part from the clean cake was comined with fresh LT to do a test reboil so as to better gauge the disolving props of the LT on pseudo and as next step for further cleaning.  Well like an idiot, the precip from this step got combined with the final dirty collection of the bastard stuff still in the funnel. SWIW did note that the second cleaning wasted pseudo.  The Leverage here comes from the mostly dry ISO, (Denat, will try w/out it next), and the mix of the LT holding on to the denaturants with just enough acetone present in the LT to allow the Gaack to start it's thing, but it can't quite get a grip then it is rinsed away with a little xylene. The Still clean and dry half of the first pull was run in a semiwet PIE that lost it's lusteraround hour 5 and was worked up with a shot of TCE and a splash of jap before a final xylene rinse. Filtered again. Then based fisrt w/NaCO3 then small aditions of NaOH.  Pulled 3x xylene (yellow tint remained even after boiling) rinsed 1x h20 and 1x brine solution (yes brokedown and went to store!) split the combined pulls part 1 gassed beautifly via hcl/CaCl the 2nd portiion titrated with a hint of yellow-to-red-to-green coloring of np. Titrated product was clean but not as clean as the gassed.  After drying, gassed product left no trace on glass even when scortched to flamable stage. Poof!   Titrated collection needed 2xrecryst to reach this point, however after a 3rd rextl from water was more potent. (duh!)  Back to the Bastard tainted psuedo.  Added to a portion of ISO and repeated begining precip steps. Every time step was performed the solutionbecame more viscous and a deeper shade of yellow to orange.  The amont of psuedo seemed to drop only a little.  After a PIE Orange Gacck proudly devoured the results at the end.

In conclusion, SWIW isn't sure if the orange was defeated in the begining or removed pre-basing at the end.  Control group splips the mind in such excitement.  What stood out in SWIW's mind was the purity of the pseudo in such a short time with high yeilds.  Being a pessimist swiw opted to try and clean it up more thinking the high yeild was due to a trojan foe. Had SWIW not of TCE the end PIE solution swiw would have a better view.  With the second pie producing such a high amount of orange SWIW is left to ponder the steps, and without accurate notes and an ongoing notation of even the littlest variations, well!

So this is the addition to swiws recollections of dreams that will be fine tuned and hopefully result in 3 possible solutions. Oh for Fuck Sake forgot to talk about the LT that had been prewashed with brine 3 times...later this is way long enough! out!

Oh ya Pie results: 1st 8.00 in 6.12 out
                   2nd 8.00 in 3.60 out

           

[geezmeister]

Those are good results from your first reaction with that pill source, suggesting the merits of your extraction process.  Thanks for the writeup. It is sufficiently detailed to follow your logic and processes. I need to complete some work on a process I haven't posted about yet, but I want to give this a try.

Don't assume that the enemy is still OII gakk. I think there is a new variant on the market now that has a little different solubilities than OII and is just as yield stealing. Its time, cowboys. Its time.


but it has been stealing yields over my last four reactions. The final acetone rinse remnants do not behave like the remnants with OII present, they have a di

[gluecifer69]

Great write up weazl!

was worked up with a shot of TCE and a splash of jap before a final xylene rinse. Filtered again. Then based fisrt w/NaCO3 then small aditions of NaOH.  Pulled 3x xylene (yellow tint remained even after boiling) rinsed 1x h20 and 1x brine solution (yes brokedown and went to store!) split the combined pulls part 1 gassed beautifly via hcl/CaCl the 2nd portiion titrated with a hint of yellow-to-red-to-green coloring of np./

Sounds like Gluecifer has a new post rxn workup in the works.

[weaz1dls]

Thanx Glucifier, Swiw just read the quote in your post and realized the (yellow color remained after boiling,) refers to the boil of the pie solution after filtering out the rp.
The placement of that statement could be taken as the xylene pulls were boiled.  Maybee if it were naphtha SWIW would boil it.  When SWIW uses Naphtha or VM&P it is jolted in short bursts in the micro.  With intermitant swirling.  Funny how it is the np layer, when ladened with honey and or atop a strong basic solution is suddenly not so invisible to the microwaves. It has been SWIW experience that this is the perfect set of variables to break honey free and keep the VM&P hot durring rinsing.  Careful though cause the upper part of the glass container will be put under high temp changes vary quickly as the bottom stays cool.  5-8 sec on, then with gloved.mitted hand swirlit round.  Don't be ginger with it however it's not a frapachino, so try to keep the reciprecating/frothing back and forth movements to a minimum.  Also one would expect that if you covered the opening and mixed it or even shook it up it would build pressure and need to be vented, spraying each time.  In fact it creates a vaccumme as the hot np mixed with the cooler lower aqueous layer we see the oposite result as witnessed when hot water layers are mixed with cooler np layers.  The np transmits the heat by expanding and creates pressure.....
                    Oh for cryin out loud SHUT UP!...
  Then one year at band camp....

[gluecifer69]

but it has been stealing yields over my last four reactions. The final acetone rinse remnants do not behave like the remnants with OII present, they have a di

Swim wasn't sure what Geez meant by this.  We know Geez has no problem with spelling or grammar so I assume it is some sort of typo.  Not being an asshole just wondering for clarifacation.
Does anyone think the yeild stealer could be (-)(-)psuedo ware has been warning us bees of, or would it be required to be listed.  Obviously the orange 2 gakk is not listed.

[SHORTY]

And other polar liquids than they do on non-polars.  Actually, they don't have any effect on a non-polar liquid.  But they will usually heat the container that the np is in or any water that is in the np.

[geezmeister]

Glucifer: I meant to say the two gakks have different smells when you evap down the rinse acetone. I don't know for certain what happened with the rest of that sentence.

I am hearing from others who have a noted a change in gakks again, and in my experience thus far, what I take to be a  new form of the OII takes a heavy toll on yield. I had too many variables involved in the last reaction to draw any conclusions from its results, so its back to lab to do it with a one-variable-at-a-time methodology.

[wareami]

weaz1dls: Excellent work dewd. The process used is vastly different than the ones Ibee's been experimenting with that utilizes  LacquerThinner.
There is no doubt that a small portion of pfed is dissolved in the LT. Most probably taken UP by the methanol.
More extensive work needs to be done in areas concerning solvent ratio/solubility versus concentration/saturation of both GAAKs and pfed.
Just like in the IDEA Method, a balance can be attained that discourages the pfed from traveling with the gaaks into solvent. This was done by ratio adjustment that took advantage of competition between the pfed and gaak
Anytime more than two solvents are used it becomes more difficult to finetune depending on solubilty.
A write-up from UP-AWE-NITE has been stalled until the newer LT formulation can be aquired and employed.
The stuff Ibee used in past experiments seems to have been discontinued but should still be available at smaller mom and pop hardware stores.

Does anyone think the yeild stealer could be (-)(-)psuedo ware has been warning us bees of
gluecifer69: When that formulation hits the shelves, there will bee no mistaking it's presense. Sad but true!
They have the patent for the -(-)pfed but I suspect they'll have many legal hurdles before they can employ it.

I am hearing from others who have a noted a change in gakks again, and in my experience thus far, what I take to be a  new form of the OII takes a heavy toll on yield. I had too many variables involved in the last reaction to draw any conclusions from its results, so its back to lab to do it with a one-variable-at-a-time methodology.
Geez: The Kidz have to concur about a new beast in the pfed hood. And it's coincidental that they've had too many variables that coincided with the last  runs to blame it on a specific gaak being the root cause.
They've recovered close to the expected yield in the last 2 runs (minus stuck on glass wastage and such), so if it was a new gaak causing the problems, it was tamed somewhat by the frontside extraction treatments.
We'll know more soon