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idea for obtaining freebase..

Migrated topic.
Hmmmm.....

Nobody jumping in to give advice....

Forging ahead!:lol:

I'll add 25 more grams of sodium carbonate hoping to get to ph 10 at least, then start dry IPA pulls. Will post results soon.

Pokey


Edit: Added 50 grams, 25 at a time, ph is 9.4... I don't understand why there isn't a more direct relationship between quantity of base added to ph. Time for some internet research I guess. Solution still looks just like milk. Weird.
Since the solution is totally opaque, I can't see if the Na2CO3 is collecting on the bottom or mixing in. Will root around in there with a spoon and see what's going on.

Pokey
 
Well I added 100 ml of dry IPA and mixed thoroughly.

Not looking too promising so far. Been over an hour and no sign of seperation yet. This process has filled my head with questions.

Why don't I get an exciting reaction when adding boatloads of lye to my acidic MHRB soup in other extractions? Isn't the rapid change of ph what makes the vinegar/baking soda experiment so frothy?

If IPA and water can mix, why wouldn't the dry IPA that I added to pull just mix right in with my solution (I think it has actually)? Is it because the ph of the solution is really high? If so, how high does it need to be to keep the IPA from combining with it?

If IPA or acetone pull full spectrum alkaloids, why not use one of them in place of the d-limonene. BLAB is the cat's ass for obtaining DMT-fumarate, but if one wants full spectrum freebase, is there a way to pull it right from the basic mixture instead of acidifying, basifying, acidifying again to salt, basifying again before pulling etc...

Where are all the Blue Flask Folks? I feel a little lost in my experiment, and am wondering what to try next. If no one feels like giving advice, I'll probably base the shit out of my solution with lye and see if the IPA seperates. If not, I'll probably bag it and pull with heptane. Chalk it up to a good idea attempted by a bad chemist....


Pokey the Persistent but Slightly Discouraged
 
ok wait.. to get something straight first.. you added 100ml of dry IPA to what exactly? to the limonene pull? I dont understand, sorry.. or to the basified water with alkaloids?


as for the frothy, no its not just pH change, its CO2 being generated by the reaction between sodium carbonate and acetic acid...
 
I added it to the basified solution. The D-limo is tucked away in case I screwed something up and the DMT is still in there:wink:

Didi you read the las posts on page 1? I think I went through everthing I've done so far.

Thaks lots for replying! I really appreciate the guidance.:d

Pokey
 
IPA and water are miscible.. for them to separate, the water layer needs to be really saturated with sodium carbonate.. so I guess your best bet is to throw tons of sodium carbonate in there, no worries if its supersaturated and there is undissolved sodium carbonate.. thats what I would do at least, hoping the IPA will separate then... in the laaaaaaaaaaaaaaaast case if it doesnt work, the whole mix can be put open to evaporate, the IPA will evaporate first and this will leave with the alkaloid-full water which can be pulled with limo again once there is no more IPA

so from what I understand, this is only the first vinegar pull that you did on the limonene, and then basified right
 
I did 2 300 ml pulls, both pulls were mixed relly well several times before seperating. I'm headed to the "lab" right now to add more sodium carbonate! Do you have any answers to my ph questions? I don't understand why the ph isn't maxed already with the amout of sodium carbonate added already. The testing I did on plain acidic water with the same ph, but no alkaloids was very different. Brought the ph up to 10 with less than 10 grams. Weird.

Thanks Again,:)

Pokey
 
yeah you did 2x 300ml limonene pulls, yes? but then you only salted with vinegar one of them, and this one salted pull is the one you later based and then added the IPA, right? sorry if im taking long to understand..

as for the pH, im not so well versed in chem to know exactly about the question you asked, but I guess it has to do with equilibrium being changed by the other ions and substances in the water.. we'll have to wait for one of our chem experts to answer this one
 
I did 5 100 ml pulls with d-limo. Then 2 "pulls" from that 500ml of saturated d-limo of 300 ml each: I added 300ml of ph 2.4 water/vinegar solution to the 500ml of d-limo, shook like hell, let it seperate, shook like hell again, etc.. 4-5 times. Then seperated the acidic water and did it all again. Ended up with 600ml of water/vinegar/DMT salts (I hope!). Then started adding the sodium carbonate as described above.

Thanks for your patience.

Pokey
 
ok now I understand, thanks :)

so the bulk of your alks should be there... dont throw anything away if it doesnt work as expected, heh?

but yeah try the excess sodium carbonate thing and hopefully that should work.. report back ! I might take a visit to some 'elf friends' tonight, if you know what I mean, so I might not answer, but if so, tomorrow Ill be back :)
 
Wow! Crazy stuff going on in Pokey's lab tonight! I added a BUNCH of sodium carbonate to the mix and shook like crazy. There was some (not alot) that wouldn't mix in, so I assumed I had reached maximum saturation.

I checked about a half hour later to see if the IPA was seperating and it looks like ALL of the sodium carbonate is sitting at the bottom of the jar. Like it all crashed out of the solution somehow. Very odd. I will decant the solution and see how much is there, but I know it's most of it just by looking at the volume. There's like an inch or more in a solid layer.


Pokey
 
IPA is a poor choice with salts and this is an example of why.
When making black powder one makes a saturated solution of KNO3 mixes the sulpher and charcoal into this and mixed well so the solids are completely wetted. This is crashed with IPA so the oxidizer is as fine and as permeated into the others as possible.the solids are filtered from the IPA and water and dried.

Wow! Crazy stuff going on in Pokey's lab tonight! I added a BUNCH of sodium carbonate to the mix and shook like crazy. There was some (not alot) that wouldn't mix in, so I assumed I had reached maximum saturation.

I checked about a half hour later to see if the IPA was seperating and it looks like ALL of the sodium carbonate is sitting at the bottom of the jar. Like it all crashed out of the solution somehow. Very odd. I will decant the solution and see how much is there, but I know it's most of it just by looking at the volume. There's like an inch or more in a solid layer.
Click to expand...

In this the IPA crashed the carbonate and is now in solution with the water and the alks are still trapped or worse landed in the carbonate pile.At this point you can still retrieve it with several naphtha pulls and probably will not be able to precipitate the base due to the IPA but evap should yield something.
Good Luck!
SB
 
Thanks Soxy!

I was ready to pull the plug on this experiment anyway. I WILL retreive the goods! I may not be a great chemist, but I'm very persistent.

Pokey the Unfazed
 
Well I was using it with salts, right? The slightly acidic "pulls" from the d-limo should change the DMT base to DMT salt which is why it moves from the d-limo to the acidic solution. Then pull from that with dry IPA. At least that's how I understood it.

I may not be the best chap to be trying new techniques as I'm still quite a novice! I was also working with materials that were new to me- sodium carbonate I've used for washes, and dry IPA was totally new to me, so I may have screwed up several different ways. I don't really like the process for drying the IPA, because there was no way to tell if it worked. I filtered it through anhydrous magnesium sulfate twice and it lost the right amount of volume, but how do I know that it lost just the water and not some water and some IPA leaving some of the water in there?

Also I didn't (and still don't) really understand ph. Well I do understand the basics, but why does the change in ph vary so greatly? I added 7 grams of sodium carbonate to 300ml of water with the exact ph of my solution, but when i added 6 times that amount to twice as much fluid volume (plus alkaloids), it didn't go up nearly as much.

So my conclusion is that the process may work just fine, just not for me this time!

I decanted the solution leaving a solid chunk of sodium carbonate firmly adhered to the bottom of the jar and based the hell out of the solution with lye (unlike many others, I have absolutely no aversion to using lye). Then started pulling with heptane. I know I won't get full spectrum freebase using heptane, but I'll probably pull with either d-limo again (if I decide on jungle salts), or toluene (if I want jungle freebase) after I'm done pulling with the heptane.

I did notice something else odd. After mixing the heptane in and letting it seperate, there was a layer of clear crystals at the bottom of the jar. I poured off the solution into another container and dumped a few of the crystals into my hand. Very, very clear and large. No idea what they were, so I crushed 'em up and put 'em back in the solution. Weird!

Will post final results!

Pokey
 
Just popping my head in for a bit: So the IPA causes the sodium carbonate to crash out of the solution like how phlux uses acetone to crash out alkaloid salts and other components? When moisture contaminated IPA (~10%) is added to some alkaloidal salts, it forms droplets of saturated water along with supernatant. To test whether this will work without using actual extract, take a bit of vinegar, mix in some sodium carbonate with some vinegar and add IPA (no wories about drying, as it's only going to come in contact with more water, and whatever % water is contained will separate out if it works). In any case, try freezing the mixture to see if the moisture settles out as ice.

Edit:
The bottom layer won't freeze, but separation seems to occur with two distinguishable layers.
 
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