No reaction in my rxn - what the heck?

[fearnoevil]

Swif just went thru a lengthy extraction of his pseudo - did a TCE/JD extract, ended up a gooey mess wouldn't dry after 2 days, followed Wareami's instructions and tone washed, LT washed w/several steps to remove oily gakk, tone washed X2 to remove remaining blue, ended up with 5.5g E after starting with possible 14.4g (but Swif spilled about 1/3 due to ghetto-funnel-holder-failure   ).

Followed the SOP for a Short/Dry rxn verbatim and mixed:
5.5g pseudo
4.4g RP
6.6 I2
1.5ml DH20
Mixed pseudo and rp first then added DH2o then added I2 (chopped this up with a razor first, small amount melted and stuck to razor? but tiny amt).

Swirled/mixed then put in ice bath, chili melted a bit, then after 10min took out and left for 15min at room temp, chili got a little more muddy but no smoke.

Put flask in sand and oil bath at 150f, chili melted and started to bubble slowly, chili seemed a bit thick (but then Swif has added too much H2o in his 2 previous attempts) balloon filled to about fist-size, still no cloud, smoke nada. Continued heating for 30min raising temp to 180f, balloon expanded a bit more, bubbles still going, but never had big initial event, and no swirling cloud as in previous trys.

Swif should mention that at one point the tip of the thermometer got moved and was not stuck into the sand - never used sand before so didn't think much of it but then he noticed that the temps were dropping. Swif turned up the heat but after 10 min when temps seemed low raised it again.  Few minutes later wondering if there was a temp differential he pushed the tip to the bottom of the sand and the temp shot up from 190f to 275f!!! The flask/chili had probably been in the higher temps for about 12 min Swif guesses and he hopes this didn't burn up his goods.

But now Swif began to suspect insufficient/weak rp as a possible culprit???
So after another 20min of this he decided to add 1g of rp. He held the rubber surgical hose clamped in his teeth    to maintain balloon pressure, opened flask and tossed in rp then closed it up.

The chili seemed to dry up immediately and bubbling stopped, but returned to oil bath. After maybe 10min like this chili was still dry and nothing was happening and Swif figured maybe needed more DH2o and since no rxn also decided to add more rp and I2   . Repeated above procedure, added the remaining .7g rp (total 1.7 extra rp), 2g I2 and 1ml DH20.

Back in the bath chili liquified and Swif thought he saw the slightest puff of smoke for a second, but then chili started to just make small bubbles again??? Seemed a bit too liquid now (shit again!), balloon expanded a bit more (about grapefruit sized), lots of redish sweat trickling down sides of flask.

Over the next hour raised temps to 225f then upped it to 250f. cuz Swif figured he's now got too much h2o and so maybe ought to run this more like a long wet rxn (maybe medium semi-wet rxn). He's read somewhere where temps should be about 115-120c so that's why (he wasn't absolutely sure about this). The entire time Swif can see lots of little bubbles comming up outta the chili so he hopes this meant something was happening.

After 3hrs of this shit, and not having a clue as to when this will end, that is IF anything is actually happening and he's not actually just been watching steam boiling out of a dead batch of chili, Swif decided to leave the kitchen and head to his den and ask for some input. Swif didn't find any answers that nite and, having to work in the a.m., he decided to sleep for 4 hrs. and then ck to see what happened.

SO, any ideas as to WTF went wrong and what, if anything, is actually happening at the moment? Swif would sure appreciate some insight to what went south on his rxn. Thanks in advance for any help!

P.S. Is it ok to leave the stuff cooking unattended for a few hours? Swif left temps dialed in at about 115-120c, and fire saftey measures are in place 

EDIT: Swif took a nap and woke up 4 hrs later  and went back to the kitchen. The chili was now slowly making big bubbles, red sweat was replaced by clear condensation, liquid in chili looked clear to just slightly yellowish.

After removing from heat and cooling, opened and smelled some kind of chemical, petro oil smell, not at all like fish??? After adding DH2o and rinsing rp Swif found lots of little round white globs that had a hard rubbery texture like plastic, ?WTF? mixed in with the rp!!! Don't see how that's possible but it resembled the white plastic tubing he uses, tho the plastic didn't look like it had melted. Is this some kind of gakk that cooked out or is Swif crazy and it is plastic?

After filtering x3 the liquid is almost clear like water, only slight tint of yellow but very faint. Doesn't look Swif thinks - he wonders if he should go ahead with the rest of the process or is he right in thinking that, without the proper signs this is just a fucked batch and he should just start over? Thanks for any help, it's appreciated  

[The_Animal]

If all the orangeness from the I2 had definately gone and there were no signs of orange whatsoever, kewl. Being clear is also a good sign. swim has had 1 or 2 cooks that no matter how long they cooked for, the slightly orange tint to the clear filtered reaction fluid usually meant a bit of a clean at the end.

Work it up

[fearnoevil]

Yeah it was clear as water, no red which Swif thought was cool, but the smell seemed to say different. Now understand that Swif's not actually had a sucessful rxn (2nd try produced maybe 15% product mixed with gakk and pseudo, lol), so he doesn't "know" the smell but everyone says it's fishy and this didn't smell like seafood, more like leftover sludge from the Exxon Valdez   .
Yep, Swif supposes he needs the practice even if nothing comes of it so he's off to his kitchen to see what's up. Will post results good or bad, wish Swif luck!

[wareami]

....says listen to The_Animal
The fishy (catpiss)smell is only present during the basing stage.
Finished rxn smell is very similar to satan's ass!
Unmistakeable!

[the_wasper]

starts as soon as you start adding chems and if you let it go for 3 hours with the ratios you supplied you more than likely  completed the recuction so Ibee would finish what Ibee started.Being new at this you definitely need the practice and don't worry swif will get good at this in no time, you are already off to a great start by joining this discussion group.

[unionpacific]

You'll only be able to smell the amine smell when dealing with bigger amounts, small scale you'll probably only smell the NP when you base. (right?)

[fearnoevil]

First off thanks Ware, yeah swif was at the kitchen and rereading his guides when it hit him that the fish smell didn't come til later, lol! Not sure what Satan's butt would smell like (tho maybe he'll find out some day, heh heh).

Wasper, ya being green as new grass has some definite drawbacks not knowing what to look for, but truly Swif's glad he found the hive and hopes to beecome a good worker bee some day ;?D!

Well right now Swifs too twisted to do this up right and he's having a hard time remembering exactly what he did and saw cuz it was pretty confusing at times (plus his brain is baked, but more on that later) but he'll try to cover the essentials.  Talk about some strange shit, swif's run into if tor sure tonite.

Swif went ahead and followed Geez's Post Reaction Workup. Everything went well, did the Non-polar solvent wash of  filtered honey, 2 of xylene and one hot naptha (since extracted with TCE would have preferred a wash with it but was all out   . The washes didn't seem to pull much but the xylene washes made the rxn fluid cloudy, but that cleared with the hot naptha.

Went with the a/b and that's when shit got wierd   ! After putting the aqueous sol and naptha in the sep funnel (only had 5.5g E to start so figured only add 100ml nonpolar) he started to add the NaOh - oh yah ck'd the ph of the sol first, it was around 1.  Started adding base but each time he put drops in, instead of the sol going cloudy, it looked like the lye turned into lots of little white solids and sunk to the bottom. Had to swirl a bit to get these to disolve.  This went on for some time and after adding maybe 2ml of lye, ck'd ph and it was still around 1!!! Methinks swif created a VERY strong solution of HI!!! 

Started adding about .5ml at a time and can't remember how many times but lots and the ph was only up to 6/7 AND swif could see orangish looking shit forming in the middle AND the solution started to turn blue!!!  Continued adding more and the solution ended up being dk brown almost like coffee before swif finally lye locked it.  Adding hot DH2o got it back and seemed help get rid of some of the emulsion AND swif finally smelled the fishy odor, so he had some hope, tho the wacked appearance of the aqueous sol flipped him out! He added about tblsp of rock salt and followed Geez's directions.

Went and added some acetone and this pretty much got rid of emulsion and so he decanted sol and then separated the two adn swif saw that the nonpolar had a very faint blue tint, grrr. At this point swif decided to only do the one pull in case the whole thing was a waste of time (it was getting late too), but saved the sol for later. 

Did 2 washes with DH2o, noted a slight slippery feel and decided what the heck and did a lye wash followed by another water wash.  Naptha STILL had a very faint blue tint but at this point Swif just wanted to get the suspence over with and see if ANYthing was in there.

Swif then gassed the naptha and the first time yielded almost nothing, just about a dime size film of white dust, BUT Swif was extremely happy to see that there was something in there.  Well he couldn't wait and so went ahead and bioassayed the whole thing. Why? Well he never did get that GOOD rush he expected, even tho in the back of his mind he knew it would be better to finish cleaning/re-xtling the stuff.  Also it was gakked (which he figured would be the case due to blue color, sigh).  Melted then crystalized but seemed to have something mixed that didn't make crystals. Small amounts seemed to burn fairly clean but the main lump turned brown/black when finished. Had some taste swif's used to but also very bitter??? But he did get high and is even now (bout 3hrs later), but it's a kinda wirey, hollow, jaw clenching feeling   .

Went ahead and gassed 3 more times, each time got about 3x amount of first gassing.  Haven't weighed it but it might be about 1 1/2g's, but of course thinks more than half of that might be gakk, but won't know til tomorrow as Swif needs to TRY to get some rest for work. He'll ck back first to see if you Master Bees can tell swif how to get rid of the gakk if it's possible. Thanks much for your help, advice and words of encouragemnt, it is greatly appreciated by this apprentice bee  

[jammin]

Thats a relief.... hehe

How much freebase (educated guess) do you need for the fishsmell to overcome the NP (in my case toulene)?

[unionpacific]

" Small amounts seemed to burn fairly clean but the main lump turned brown/black when finished."

That's unreduced ephedrine or gaak, I'm guessing the part that turned brown/black looked like the surface of toast?

re: jammin
I've only had limited experience with toluene I don't really remeber what it smelled like before I used it. Perhaps my nose is fucked up, but in my experience with xylene and naptha anything over ... uhh around 7 grams or something depending on how much NP solvent your using to pull the freebase will give me that fishy amine smell, imagine how much it reaks if your doing a A/B on a larger scale!  

People have actually been busted by this fishy amine smell. Wouldn't that suck to have a pyrex evap dish on a hotplate with some ounces in the water and L.E start knocking on your door,(quick, get the brownie mix!! ) all the work gone down the drain because of strong amine smell when basing.

[Shane_Warne]

'How much freebase (educated guess) do you need for the fishsmell to overcome the NP (in my case toulene)?'

They're talking about the basic water, with the freebase sitting on top.
not from within the toluene or NP.

Clear is good because it means that the recycling agent is actively reconnecting all the H's and I's swimming around in to HI.

but it doesn't describe the concentration, just that the rxn solution contains pretty much all HI and no free I2.

Practically speaking it makes the job of increasing the concentration easy, also just knowing what is going on.
e.g.
if you note a progressive and worsening discolouration of the rxn fluid, you know it might be a cool idea to add a bit more recycling agent.

if you subsequently want to test what your recycling potential is now and increase the concentration...then you would add a bit more I2 until the rxn fluid failed to clear itself.

Obviously the point at which it fails to clear itself isn't necessarily ~57%, it's just the best ratio of I2 relating to the other reagents.

If you add more recycling agent and repeat the process with the I2 additions then you'll be getting closer. THAT's IF YOU DONT ADD MORE WATER AGAIN LIKE A GOONIE.

Just in case you didn't know.

nice job cleaning your pfed mess, ~30% isn't too bad considering...

[fearnoevil]

Well Union, I'm thinking it's some kind of gakk, cuz of the bitter taste - Swif's smoked E before and it wasn't like this.  Plus Swif's STILL got the jitters and hollowness which is pretty ganky he has to say, but it sure kept him awake and horny all last nite (tho couldn't get his limp dick to cooperate at all, lol).

Still lookin for any answers on how, if it's possible, to get rid of the gakk AND has anyone else seen their rxn sol go dk brown when basing?  The blue color of the naptha must be indicator of gakk, yes?

[fearnoevil]

Shane,
Sorry, but aside from being extremely fuzzy headed due to having bioassaying his gakked meth this a.m. (it's been going on for quite awhile still, sheesh), Swif really is a greenhorn and is having trouble understanding the following:

"if you note a progressive and worsening discolouration of the rxn fluid, you know it might be a cool idea to add a bit more recycling agent. if you subsequently want to test what your recycling potential is now and increase the concentration...then you would add a bit more I2 until the rxn fluid failed to clear itself. If you add more recycling agent and repeat the process with the I2 additions then you'll be getting closer."

So are you talking to the prob Swif had with the a/b and his aqueous solution turning dk muddy brown? Cuz if so he doesn't understand adding I2. If your talking about something altogether different then feel free to boot Swif's dumb ass, lol.  Tho Swif has his bright moments, this is not one of them - could you please explain the above statements like you were talking to a 6-yr old, cuz that's about his mental capacity about now.  Thanks for your advice!

[Shane_Warne]

Let this explain.

Hydriodic acid solution

Properties:  Colorless when freshly made, but rapidly turns yellowish or brown on exposure to light and air. This discoloration can be prevented by the addition of about 1.5% hypophos phorous acid (H3PO2). Concd solns that have been stored for some time are usually opaque from oxidation, they may be regenerated with hypophosphorous acid: Foster, Nahas, Jr., Inorg. Syn. 2, 210 (1946).


Nope, I was talking about the rxn itself.

When there is discoloration, brown, red, gold it usually means that some of the HI has dissociated, to free molecules. So it's free Iodine that is currently useless.

Only when it exists as HI, a colourless solution, is it being put to use.

A solution of HI without a recycling agent will rapidly discolour.
With a good recycling agent present, the solution can maintain itself in a transparent state, for long periods. Constantly rejoining the free I and H's floating around, that have dissociated due to temperature, light and air.

So your rp looks out for I's and H's floating around and sticks them together with clag or PVA or other safe for children glue, wearing a smock or apron!
(Well you said try explain as if talking to a kiddie   )

Incidently, H3PO3 will only start clearing at 80-90+ degrees
centrigrade. Hypo is more instant.

By adding more recycling agent to a discoloured fluid, you fulfill condition 1 (in acheiving a High concentration, 50+%), that you have enough recycling agent.

By adding increments of I2 following the fresh RP addition, you are both using your RP to it's fullest potential, and increasing the overall concentration. i.e more connected H's and I's (HI) in there relative to the water present.

I mean if you measured your reagents kind of accurately at the outset, then you will be in the ball park, so too much tampering shouldn't bee necessary.

The hardest part swim finds, is dicerning between various smokes and vapours.

[fearnoevil]

Thanks for clarifying that Shane, Swif sure feels better when he actually understands the reasons things happen. Without understanding the process it's tough backtracking to find out where something went wrong and then apply a fix.

Okay, Swif's got a short list of Q's that he's in need of answers too, so here goes:

1) Swif looked at the bottle that contained the ugly "rootbeer" like NP that he did the single pull on, and SHIT he was surprised to see it was now clear with a layer of brown and black goo at the bottom (layered actually, with the black under the brown).  Swif decanted as much as possible without disturbing the goop, but doesn't know if the remaining goods (if any) are in the clear or the ugly or maybe both?

2) Swif's been trying to clean the gakk out of his meth and may be getting close, but most likely he's missing some important step.  So far since his initial tone wash he's washed the xtals in cold/dry tone again, then disolved xtals in dry ISO, reduced then added dry tone and boiled 5 min, waited till xtals reformed, filtered xtals, dried/powdered then washed in MEK, dryed/powdered then denat alch washed xtals and let sit for several hours, found crap/film in bottom of flask so decanted and left garbage (this stuff when dried was just crap, no meth) then reduced denat added tone and re-xtalled.

He tested at each step and only on the last couple steps did he notice a considerable reduction of contaminants when burned on foil. Just finished the last re-xtal but since it's late (and Swif really needs to try and get some REAL sleep tonite), he didn't try it but melted some on foil. Stayed white (didn't turn orange) and seemed to crystalize better and didn't leave much residue when burned off, as opposed to leaving a thick charred black resin as before. Course he only tested a tiny bit, since he's now down to about 1/2g from the 1 1/2g he started with, lol.  He's sure some is still in all the solvents but he just wants to get to clean the RIGHT way before worrying about the rest. Swif'll do a REAL test    tomorrow and then post results.

3) For future ref, should Swif clean his rp with murry to make sure no gakk has coated it waiting to fuck up his next batch? Swif's leaning that way but if there's better way to clean he's all ears ;?D (just worried that this FUCKING HORRIBLE SHIT might also have some super powers that allow it to permanently gakk up one's rp too, lol)

EDIT: OK Swif was just fooling himself. Burned some this morning and in larger quanities it is easy to see that it's still gakked. It initially looks better, doesn't turn orange right away and cracks back well enuf, but still has a strange/nasty taste, hard to describe, and it eventually does change color and still leaves a crusty ash. No euphoria but does have a lift but takes several big hits to get some effects. 

Swifs about to give up on this batch but he's hoping perhaps there's a cure and any advice is appreciated, TIA

[fearnoevil]

Well, Swif's still hoping there's a way to clean the meth - is it possible or just chuck it and chalk it up to experience? TIA

[wareami]

Fearnoevil: If tone washes and re-x-talling won't clean it up, than it's damn near impossible to suggest anything that might help because the cause of the contamination remains a mystery to you as well as us.
Sometimes we are all left to our own devices toward  arriving at solutions to problems that are unique to the situation we created ourselves someware down the line.
Go with what ya know.....or as you fear....as a last resort, chalk it UP to a learning experience!
Some may laugh their asses off at Ibee's initial fifteen failures, but he'll say it again:
He learned more from those failures than he would have ever learned if everything was smoothe sailing from the Git-GO!
It may sound harsh, but it's not intented.
Shit happens.
I couldn't even suggest another route of consumption without knowing for sure what the contamination source was.
Many avenues need to be examined when troubleshooting rxns or less than pristine goodz and this is what makes or breaks a bee in the long run.
Get a handle on it if you can so you'll know better next time.
Anybee that doesn't agree that learning comes at a price hasn't learned very much IMHO.

[SHORTY]

then disolved xtals in dry ISO, reduced then added dry tone and boiled 5 min, waited till xtals reformed, filtered xtals, dried/powdered then washed in MEK, dryed/powdered then denat alch washed xtals and let sit for several hours, found crap/film in bottom of flask so decanted and left garbage (this stuff when dried was just crap, no meth) then reduced denat added tone and re-xtalled

Could you explain this with a little more detail cause i fail to see how you are recrystalzing anything in the above procedure.

[fearnoevil]

Ware, can't argue with the truth :cool: , Swif is learning from every screw-up and gakk-attack, but not having any chem xp makes it a longer learning curve when he doesn't really know the different characteristics of solvents and even the lingo sometimes sounds/reads like Cantonese, lol.  But Swif is nothing if not persistent so his education will continue. One of the main reasons Swif decided to pick up this little hobby was because of the challenge it presented as well as the opportunity to simply LEARN!  Learning is fun and the day Swif stops learning is the day he's put in a pine box (tho if he has any say in it, he'll opt for cryonics, heh heh)

Shorty, well Swif's too green to know the dif but maybe just percipitated is what he meant.  Give him a few more months and he might know for sure just what the fuck he's doing, but right now he's just trying to find his ass with both hands :wink: