Nano rp/i2, steam distil. formed white powder?

[E_Emperor]

SWIMS First newbee attempts at rp/i2 nano reactions.

SWIM used a small salt & pepper shaker for the reaction flask, with a hose & balloon attached to the top.
Ratios were:     E         1.5grm
                     LG I2    1.5grm
                     MBRP    1.0grm
                     dH20    1-2 drips
The Reaction was left to reflux for 18 hours. Rxn went well.

MBRP was washed several times, dried & powdered before used in rxn.

Next SWIM did the steam distillation. SWIM made up a make shift "Still"

SWIMS "Still setup description:"
Big steam pot (crayfish size), place a bowl inside-lifted off the bottom by a couple of knifes laid flat, put on the steam pot lid placed-inverted. Pile up ice in dish of steam pot lid which acts as a condenser, and the bowl inside collects the dripping goods)

Anyway, cause SWIM is extremely low on any chemistry gear, and thought that this would "hopefully" do for now.

SWIM then added dh2o to the completed rxn flask and gave it a shake or 2 and poured it through a filter to remove the rp (repeated twice).
Then SWIM poured that (honey) into the bottom of make shift still. "The solution looked nice & honey/oil like."

The Still was prepared first by adding a solution of dh2o & NaOH-pH14

SWIM then placed his honey catching bowl inside the now boiling dh2/naoh. Replaced lid inverted-filled with ice and replaced with more ice over & over until all the goods had gone from the bottom of the steam pot to the bowl catching it inside.

That was then left to cool, before  it was pH tested. pH 7.5. SWIM was happy with this reading and left it at that.
SWIM doesn't know how expectable this setup is to achieve re-crystallization

The solution was then left to evap with the aid of a fan.
While waiting for the time consuming process of evaporating water. SWIM had a sample of the goods and took small drink... and Woooah, 30 minutes later SWIM was speeding hardcore.

SWIM was very happy, as past attempts had failed-or fucked up.
So waiting for his crystals to form SWIM waited

But what formed was a very light weight, white-ish powder, that wouldn't burn.
SWIM thought that maybe his E had Gakk in it.

SO for SWIMS next rxn, SWIM pulled a new batch of HCI-E using Methanol, washed & refilterd twice.
This gave SWIM some impressive E, long needles of glass glistening, So nice any dry much cleaner looking than what SWIMS pulled before.

So SWIM did another rxn, using the same weight ratios, and setup like before.
But only did a 4hr reflux this time, as SWIM has read so many bloody posts on rxn/reflux times and all the arguments by fellow bees about there differing views. So SWIM took a medium between the suggested times.

Hoping to produce smokable crystals this time, Since SWIM guessed that it must have been Gakked E that caused the white powder to form instead of crystals. last time.

But, it's not looking hopeful. SWIMS honey is evaping at the moment but the same thing is happening as last time. A White-ish Powder is forming on the surface and there's still quite a bit to evap yet.

What has SWIM "Fucked Up" this time! SWIM is thinking that  crystals will not form again, just this powder crap.

So assuming SWIM has told you all you need to know,. Do any Bees have any thoughts where SWIM "Fucked Up"? or any advice on what to do to get Crystals.

How can SWIM, save his Honey and crystallize it?
SWIM has toluene, methanol & acetone at his dispose.

Any advice is most welcome. Thanks heaps

Cheers E

[WizardX]

2H20    1-2 drips

H2O, not 2H2O

Are you saying you added 1-2 drops of water? If that is the case, it's not enough water.

[morpheus]

You say your using E and not psudo.What are the inerts?
What extraction method?
Wizard is right,an 18 hour reflux and using 1-2 drips DH2O,
the I2 is lab grade(anhydrous)where I2 from tinc  would have had some more water.

[geezmeister]

If you will take the time for the reaction to simmer along just under 100C for twenty four hours, why not add a ml of water for every gram of pseudo right at the start, capture all the HI the I2 and rP make in the water, and reduce the pseudo with that HI to the intermediate and then the final product? You were outside the success envelope with the dab of water you added.

You have read other methods for making methamphetamine using a very limited amount of water. They will make some meth, done properly, but invariably contain more intermediates and by products than a wetter reaction will contain. If you want the tweaky side effects, you cook hot and dry. If you want the purer meth, use more water, lower the heat, and let it simmer for 24-48 hours. Just do it once to see for yourself. That was all it took me.

The wet reflux takes longer. That is the ONLY thing I know about a wet reflux anyone can complain about. No learning curve, no sophistication, no broad knowledge base required. Does it all by itself inside the flask without user intervention. The reaction is the easy part. Cleaning the pseudo is where the work is.

Unless you insist on leaving that water out.

As to recrystallization of any meth you have, check the sticky threads in the newbee forum on dual solvent recrystallization. I doubt you will get shards in the evap dish with the methods you employ here without such recrystallization.

[E_Emperor]

Your right Morph. It was pseudo SWIM used.

Cool gezz. Yes, SWIM has read so... so... many differing & conflicting views, especially on wet/dry & short/long rxns. SWIM will take your advice and do a long wet reflux-(at least 24hours)

SWIM has just learnt more about HCI salts and importance of lowering pH (acidfy) to form crystals.

What method do you bees do to get crystals? Do you Gas or use solvents?
Any advice on this would bee awesome...

Thanks Bees...

[geezmeister]

I tend to titrate and evaporate, flash with acetone, rinse with acetone, and then dissolve in alcohol, filter, reduce the solution to saturation, add acetone, and chill. I take the crystals formed by this process and dissolve again in alcohol, filter, reduce to saturation, add acetone, chill, and harvest the crystals. If you want cleaner meth, don't chill, let the temp drop slower, let the crystals grow slower. Keep working the mother liquor until it gives no more crystals. Put it in a cool, dark place and check it again in a few days. If you gas, the process is the same.

I have shards after acetone flashing. I have crystals after dual solvent recrystalization. I am not sure which one you are referring to.

[Ganzas2003]

I think that after the tritration one should get a burnable product, dispite of dirty or residue. If it doesnt burn recristalization will not do the miracle. recristalization is a cleaning method. its not a way of makin shit smokable if u can understand what im saying here. SWIG got that problem once...but back that time he didnt understand shit of what he was doing as he was only following the paper and he didnt wash the NP solvent...which IMHO i think it's VERY IMPORTANT. Shit was white...shiny/glassy at some point, but it didnt burn...not even a little. SWIG got fukin demoralized coz back there he thought: " jesus lord!!!so many fukin shitttttt...uhhhhhhhhhh!!! Ive done it this time!!!" but no...it didnt burn...lucky this was the secong reaction vessel water pull  so some product was still enjoyed.
SWIG has 4 reactions till now. all nano 1-2g . allways felt speed.allways got product.
Of course, now SWIG acts very diferent... to the best!!!    and he can only thank this site for that....twice actually, as this site told SWIG about makin drugs and  its teaching him along the way!

thx.
peac.


Peace!

[Relux]

I have a small tidbit to add to this, and tell me if I have just read wrong, as the bezodiazepins are starting to kick.

Anyway, it looked to me that after the steam distillation (I'm assuming you both obtained water and *freebase* oil in the collection basin) you took the distillate water oil and all and went to distill it strait away. My confusion is: did you acidify before you started evaporation? if you haven't then you will have the freebase oil that will not for crystals. I don't understand how you came upon getting any solid from the distillate other than the sought product, but there is just no form of it that I have ever heard of that doesn't burn.
I'm no master at this, but someone who isn't Re did a nano for the fun of it the other day and did it no prob.
My brief: barely touched the pseudo red hots (methanol, evap; base/acid, evap) so it was kinda gooey (red and chewy). Threw this is with some funky mbRP and polar pure with a few drops of water (c'mon people, this rxn makes water so not much needs to be added for these little crap shoots) a few more drops of water were added to semi-de- solidify the clay mass that had formed after the rxn had to be stopped for a bit. Stirred for 2hrs under reflux. 3 base extracts (naptha), 4 acid extracts (tH2O (that's right, t=tap) with concrete cleaner. Dried extracts on a plate, scraped them up, recrystallized in 99%isopropylalcohol to lustrous white flakes/jagged/tablets. Odor, none. Burns to nothing. Smokes smells just right. A dab was stolen, reported as the bomb. A dab was mixed with base, bubbles of oil floating to the surface with rauchy honey odor. No doubt good shit from a barely tried run, melting range 2 degrees off , but hey- my thermometer sucks.
Anyway, sorry to blab, I think that all you need to do is acidify the distillate to get your crystals. The unburnable white solid I would think was some salt of neutralization present but hey! I thought you distilled this shit??
Whoa man, my head is spinning right now, so I hope that was of some help. Lorazepam I love you!